High yielding trans-2,5-Dimethoxy-beta-nitrostyrene synthesis (detailed description)
- Thread starter FENTAMAS
- Start date
Okay @FENTAMAS,
Fair play to you - I at least quadrupled my yield by simply keeping the filtrate and following your instructions. I’m still just filtering the last - I added EVEN more water and got EVEN more precipitation, even when I really was not expecting it and thought the RM was done.
Given how much more I got out of it by simply adding water and keeping cold, I’m guessing if I had kept the last RM and done the same i probably would have gotten even more from it. The only reason I say that was its willingness to crystallise even at high temps like 30c - that was really incredible!
I also learned make sure you chill everything you are washing wish in the freezer…
I’m not far from being out of the starting aldehyde - although I could obviously get more and maybe I will BUT I have some 3,4,5-trimethoxyBA coming in bulk instead.
I figured I’d give the reductive animation of cyclohexanone a go and then if I can’t manage it as the paper suggests, I’ll just buy it from my friend who can order stuff from sigma, I guess. That’s where the ethylenediamine came from for this RXN - same goes for everything actually now I think of it - other than the GAA…
Anyway as always I’m rambling but I just wanted to say a sincere thanks.
I’m currently working my way through the books ‘organic chemistry as a second language’ the thing is I’m also doing a BA hons in Art and so I’m probably going to have to combine the two and make some pigments to be honest.
Then use them to write an essay about or use them to paint with. We’ll c…
I love how versatile chemistry is though, if you have any interest, it almost certainly contains chemistry at one point or another.
Fair play to you - I at least quadrupled my yield by simply keeping the filtrate and following your instructions. I’m still just filtering the last - I added EVEN more water and got EVEN more precipitation, even when I really was not expecting it and thought the RM was done.
Given how much more I got out of it by simply adding water and keeping cold, I’m guessing if I had kept the last RM and done the same i probably would have gotten even more from it. The only reason I say that was its willingness to crystallise even at high temps like 30c - that was really incredible!
I also learned make sure you chill everything you are washing wish in the freezer…
I’m not far from being out of the starting aldehyde - although I could obviously get more and maybe I will BUT I have some 3,4,5-trimethoxyBA coming in bulk instead.
I figured I’d give the reductive animation of cyclohexanone a go and then if I can’t manage it as the paper suggests, I’ll just buy it from my friend who can order stuff from sigma, I guess. That’s where the ethylenediamine came from for this RXN - same goes for everything actually now I think of it - other than the GAA…
Anyway as always I’m rambling but I just wanted to say a sincere thanks.
I’m currently working my way through the books ‘organic chemistry as a second language’ the thing is I’m also doing a BA hons in Art and so I’m probably going to have to combine the two and make some pigments to be honest.
Then use them to write an essay about or use them to paint with. We’ll c…
I love how versatile chemistry is though, if you have any interest, it almost certainly contains chemistry at one point or another.
That's good you got the rest in crystalline form, but your last crops better hold separately, do not combine them.
If you have some time, try to recrystallize that last product you get to simplify its identification.
I have serious doubts that it's entirely 2,5-DMNS, as it haven't such great solubility to remain so well in your freezed solution.
There is a big chance that your aldehyde is mixed with something else.
I know that your supplier sent you many good quality products, but there is big difference between common simple and cheap reagents that are mass produced in the industrial facilities, and direct or indirect drug precursors that have negligible legit use, especially if we are talking about black/grey markets.
That's why I noted about preliminary quality check in the first place of this synthesis. Chemists often purify their reagents before syntheses even from well-known big suppliers, so in this environment you can't trust anyone's word.
Such technique as checking the melting point is very simple, especially for low melting materials as this 2,5-DMBA.
If it starts melting at least at 45-46C and fully liquefies within +2-3C range, then there is chance of acceptable purity.
Take some video-instructions of how to make this right. Thin glass capillary tube, stirring, slow heating rate over 40C, etc.
As I see you have already tried TLC, that's even better way to detect any adulterants, but you definitely should improve your skills and preferably get some plates with fluorescent 254nm UV indicator, short-wave UV light source (UV-C, completely invisible), filters to protect your eyes, pure solvents etc. Sorry, I haven't time to teach you this here in written form and explain each step. But you can get some good lessons on youtube, of course.
It's a bit costly, but I assure you, if you get good skills with this analytical method, your chemistry skills and reaction yields will make quantum jump from your current level after some practice with organic reactions controlled by TLC.
If you have some time, try to recrystallize that last product you get to simplify its identification.
I have serious doubts that it's entirely 2,5-DMNS, as it haven't such great solubility to remain so well in your freezed solution.
There is a big chance that your aldehyde is mixed with something else.
I know that your supplier sent you many good quality products, but there is big difference between common simple and cheap reagents that are mass produced in the industrial facilities, and direct or indirect drug precursors that have negligible legit use, especially if we are talking about black/grey markets.
That's why I noted about preliminary quality check in the first place of this synthesis. Chemists often purify their reagents before syntheses even from well-known big suppliers, so in this environment you can't trust anyone's word.
Such technique as checking the melting point is very simple, especially for low melting materials as this 2,5-DMBA.
If it starts melting at least at 45-46C and fully liquefies within +2-3C range, then there is chance of acceptable purity.
Take some video-instructions of how to make this right. Thin glass capillary tube, stirring, slow heating rate over 40C, etc.
As I see you have already tried TLC, that's even better way to detect any adulterants, but you definitely should improve your skills and preferably get some plates with fluorescent 254nm UV indicator, short-wave UV light source (UV-C, completely invisible), filters to protect your eyes, pure solvents etc. Sorry, I haven't time to teach you this here in written form and explain each step. But you can get some good lessons on youtube, of course.
It's a bit costly, but I assure you, if you get good skills with this analytical method, your chemistry skills and reaction yields will make quantum jump from your current level after some practice with organic reactions controlled by TLC.
That’s a really great response to all my ramblings.
To be honest iv started working my way through a book called ‘organic chemistry as a second language’ - I know Hamilton Morris recommends it a lot and so far it seems extremely useful but I get the feeling it’s going to take - well, the rest of my life to learn to any acceptable standard!
Oh yes, without a doubt I have collected each separate filter into a separate vial.
I actually melted some today by accident and was pretty blooming surprised at how low of a temp it started melting at! Which is a good sign I guess….although it wasn’t monitored- I was trying to just ever so slightly heat it to make sure it was dry - no idea why I didn’t just put it in the desiccator with the rest but hey.
I shall find a good YouTube video for both of those subjects but yeah, the reason for collecting everything separately is just so I can re-x each one separately.
I realised that actually it didn’t NEED the freezer at all - the fridge would have been more than sufficient to crystallise the product in so I do think it is beta-2,5-DMONS - they are still needle shaped crystals that loook very similar to the last lot just not as long by any means. They are still shards and have the EXACT same colour so I’d say it stands a good chance - especially after melting some today!
I swear I looked it up and it said something like high 90’s melting point BUT I have been doing something else since then and I may have confused the b.p of nitroethane with the melting point of this substance.
Either way I was super surprised it melted coz I was just slightly warming some silica gel beads to get rid of some solvent on them and could easily stand to put my hands in it to touch them and it still melted.
We’ll see - yes I do also need to up my TLC game but I am going to just work my way through the double semester books I was talking about earlier, first.
I mean at least I can read bloody line bond drawings now! I mean I understood the carbons but didn’t realise about the hydrogens and just the general rules!!
I like the way it goes through things in a specific order. It may not be directly related to what I’m doing yet - but everything i have learned so far from that book has been applied to the things I am doing in order to practice…so I think that’s a sensible way of doing things. CERTAINLY FAR better than bloody chatGPT
To be honest iv started working my way through a book called ‘organic chemistry as a second language’ - I know Hamilton Morris recommends it a lot and so far it seems extremely useful but I get the feeling it’s going to take - well, the rest of my life to learn to any acceptable standard!
Oh yes, without a doubt I have collected each separate filter into a separate vial.
I actually melted some today by accident and was pretty blooming surprised at how low of a temp it started melting at! Which is a good sign I guess….although it wasn’t monitored- I was trying to just ever so slightly heat it to make sure it was dry - no idea why I didn’t just put it in the desiccator with the rest but hey.
I shall find a good YouTube video for both of those subjects but yeah, the reason for collecting everything separately is just so I can re-x each one separately.
I realised that actually it didn’t NEED the freezer at all - the fridge would have been more than sufficient to crystallise the product in so I do think it is beta-2,5-DMONS - they are still needle shaped crystals that loook very similar to the last lot just not as long by any means. They are still shards and have the EXACT same colour so I’d say it stands a good chance - especially after melting some today!
I swear I looked it up and it said something like high 90’s melting point BUT I have been doing something else since then and I may have confused the b.p of nitroethane with the melting point of this substance.
Either way I was super surprised it melted coz I was just slightly warming some silica gel beads to get rid of some solvent on them and could easily stand to put my hands in it to touch them and it still melted.
We’ll see - yes I do also need to up my TLC game but I am going to just work my way through the double semester books I was talking about earlier, first.
I mean at least I can read bloody line bond drawings now! I mean I understood the carbons but didn’t realise about the hydrogens and just the general rules!!
I like the way it goes through things in a specific order. It may not be directly related to what I’m doing yet - but everything i have learned so far from that book has been applied to the things I am doing in order to practice…so I think that’s a sensible way of doing things. CERTAINLY FAR better than bloody chatGPT
Oh and as for re-x’ing reagents no matter who they are from…fair play. I shall start doing so in that case…
I assume it’s fairly easy - I’ll do it for the next reaction - I have 15g left so can do one more 10g reaction, this time having pre-re-x’d the aldehyde as well. It was a little sandy and clumpy so maybe you are right.
I have quite a lot (at least for me) of 3,4,5-TMOBA coming and so today iv been separating nitroethane from DCM this time instead of nitromethane.
I’ll probably try to make some P2NP tomorrow - something iv been wanting to try for ages…and then when the 3,4,5 comes I am hoping to be able to make some mescaline and also some TMA - it’s something iv only ever ‘bought before’ from the dark web and it felt like a hardcore dissociative - in fact my experience with them was VERY similar to my experiences with 3-meo-pcp. Black out for hours and hours and when I came too - I had savagely broken and blue toes.
So I have NO IDEA what was in them tablets but they were HORRIBLE…so I’m curious about TMA.
M first tho!
I assume it’s fairly easy - I’ll do it for the next reaction - I have 15g left so can do one more 10g reaction, this time having pre-re-x’d the aldehyde as well. It was a little sandy and clumpy so maybe you are right.
I have quite a lot (at least for me) of 3,4,5-TMOBA coming and so today iv been separating nitroethane from DCM this time instead of nitromethane.
I’ll probably try to make some P2NP tomorrow - something iv been wanting to try for ages…and then when the 3,4,5 comes I am hoping to be able to make some mescaline and also some TMA - it’s something iv only ever ‘bought before’ from the dark web and it felt like a hardcore dissociative - in fact my experience with them was VERY similar to my experiences with 3-meo-pcp. Black out for hours and hours and when I came too - I had savagely broken and blue toes.
So I have NO IDEA what was in them tablets but they were HORRIBLE…so I’m curious about TMA.
M first tho!
@FENTAMAS
I just wanted to say thanks for stressing the importance of re-crystallisation of reagents before starting your reactions.
I have come to realise the tryptamine I was working with wasn’t particularly pure because it’s now massive crystals that are white instead of like dirty tan/yellow.
When I come to do the Henry reaction again with the synthesis we were talking about here (but also when I come to do it on the 3,4,5-TMOBA I just received.) I will definitely re-x the aldehyde first this time.
Doesn’t make sense making sure everything else is super pure (like ethylenediamine and GAA) if the main reagent isn’t pure! Duh!
I just wanted to say thanks for stressing the importance of re-crystallisation of reagents before starting your reactions.
I have come to realise the tryptamine I was working with wasn’t particularly pure because it’s now massive crystals that are white instead of like dirty tan/yellow.
When I come to do the Henry reaction again with the synthesis we were talking about here (but also when I come to do it on the 3,4,5-TMOBA I just received.) I will definitely re-x the aldehyde first this time.
Doesn’t make sense making sure everything else is super pure (like ethylenediamine and GAA) if the main reagent isn’t pure! Duh!
@FENTAMAS Hey sorry, one last question…
what did you re-x your 2,5-DMOBA from to start? It seemed really soluble in methanol, I was thinking maybe some methanol and water? If you know of a better mix, please do tell…
I just tried to do a re-x of the b-2,5-DMONS from methanol first but it didn’t go too well, so I ended up looking up shulgins synth of 2c-h and saw he used IPA so Idid it from that which seemed to go better.
I just can’t rele work out what to do the 2,5 starting aldehyde from.
what did you re-x your 2,5-DMOBA from to start? It seemed really soluble in methanol, I was thinking maybe some methanol and water? If you know of a better mix, please do tell…
I just tried to do a re-x of the b-2,5-DMONS from methanol first but it didn’t go too well, so I ended up looking up shulgins synth of 2c-h and saw he used IPA so Idid it from that which seemed to go better.
I just can’t rele work out what to do the 2,5 starting aldehyde from.
Watery IPA or short-path vacuum distillation with 2-stage oil pump with fresh oil.
Use adapter as on photo below, or by connecting 2 RBFs (bulb-to-bulb distillation): one-neck flask connects to 2-neck flask and free neck via adapter goes to vacuum.
Easier way to purify it would be via bisulfite adduct, this aldehyde forms it pretty well. So that you can estimate aldehyde content in your powder, maybe it's already pure enough.
Maybe there are other preferable solvent systems for r-x'ing 2,5-DMBA, I don't remember.
As for nistrostyrenes, I wrote it from very beginning that you should use alcohol-water system.
Use adapter as on photo below, or by connecting 2 RBFs (bulb-to-bulb distillation): one-neck flask connects to 2-neck flask and free neck via adapter goes to vacuum.
Easier way to purify it would be via bisulfite adduct, this aldehyde forms it pretty well. So that you can estimate aldehyde content in your powder, maybe it's already pure enough.
Maybe there are other preferable solvent systems for r-x'ing 2,5-DMBA, I don't remember.
As for nistrostyrenes, I wrote it from very beginning that you should use alcohol-water system.
Interesting as I literally just ordered a short path distillation head!
Yes I’m not talking about the nitrostyrene’s iv had good success following your techniques re-that.
It’s more me just trying to ensure as effective reaction as possible really and trying to maximise yield.
Yeh that is what I was thinking of doing; an alcohol/water mix - am I correct in thinking I dissolve it in an alcohol and then just add dist. Water until it goes cloudy and stops precipitating.
Do I then reheat it for the aldehyde to re-dissolve and then cool down slowly or do u just put it in the fridge as soon as you e seen it go cloudy from water?
Interesting re short path distilling it - I guess that would be preffferable, except I don’t have a two stage pump - just single stage rotary vane. I did just buy new oil but it looks so different to the original clear stuff it’s probably worth emailing the manufacturer to check if it’ll be ok. Anyway irrelevant but yeh the idea behind buying the short path unit was to eventually buy a decent pump and do this sort of thing. Maybe even distilling tryptamine’s under vacuum as well for better purification but we’ll see. These things take time…
Thanks for all your help and suggestions - it may seem like I’m not following them at times but I promise I am! I’m actually so scared of losing this info I have it all saved. I know how decent threads can just disappear!🫥
Yes I’m not talking about the nitrostyrene’s iv had good success following your techniques re-that.
It’s more me just trying to ensure as effective reaction as possible really and trying to maximise yield.
Yeh that is what I was thinking of doing; an alcohol/water mix - am I correct in thinking I dissolve it in an alcohol and then just add dist. Water until it goes cloudy and stops precipitating.
Do I then reheat it for the aldehyde to re-dissolve and then cool down slowly or do u just put it in the fridge as soon as you e seen it go cloudy from water?
Interesting re short path distilling it - I guess that would be preffferable, except I don’t have a two stage pump - just single stage rotary vane. I did just buy new oil but it looks so different to the original clear stuff it’s probably worth emailing the manufacturer to check if it’ll be ok. Anyway irrelevant but yeh the idea behind buying the short path unit was to eventually buy a decent pump and do this sort of thing. Maybe even distilling tryptamine’s under vacuum as well for better purification but we’ll see. These things take time…
Thanks for all your help and suggestions - it may seem like I’m not following them at times but I promise I am! I’m actually so scared of losing this info I have it all saved. I know how decent threads can just disappear!🫥
In this case you can start right from premixed alcohol and water, then cool it slowly step-wise: to RT, then in fridge, and lastly in freezer if needed.
But your described technique is very correct, I'm glad you learned it by yourself. It's mostly used for crystallizing different salts from appropriate solvent by addition of ether.
For doing short-path distillations of substances that are crystalline at RT, preferably to have at hand heat gun to prevent clogging.
However such low melting point stuff as 2,5-DMBA could go well directly to receiving flask without problems if it's done in warm summer day with sufficient distillation rate and you don't run any water through condenser.
But your described technique is very correct, I'm glad you learned it by yourself. It's mostly used for crystallizing different salts from appropriate solvent by addition of ether.
For doing short-path distillations of substances that are crystalline at RT, preferably to have at hand heat gun to prevent clogging.
However such low melting point stuff as 2,5-DMBA could go well directly to receiving flask without problems if it's done in warm summer day with sufficient distillation rate and you don't run any water through condenser.
Oh how interesting. Yeah iv seen the heat gun used before but mainly for getting (mostly THC) out of the collection flask after it goes all goopy.
It makes sense to try and use it to stop clogging yeh.
Nice one @FENTAMAS for allowing me to learn but also pointing me exactly where to go to do so!!
Respect to you.
I actually feel comfortable following either one of shulgin’s methods for the first step of mescaline and have everything I need.
will start with the shorter of the two though! Seeing as I went to the trouble of getting the cyclohexylamine!
I’m sure I’ll fall back on ammonium acetate though tbf
It makes sense to try and use it to stop clogging yeh.
Nice one @FENTAMAS for allowing me to learn but also pointing me exactly where to go to do so!!
Respect to you.
I actually feel comfortable following either one of shulgin’s methods for the first step of mescaline and have everything I need.
will start with the shorter of the two though! Seeing as I went to the trouble of getting the cyclohexylamine!
I’m sure I’ll fall back on ammonium acetate though tbf
@FENTAMAS Have you tried this synth - only subbing nitromethane with a stoichiometric excess of nitromethane instead to form the relevant nitropropene?
I’m thinking far down the line to maybe make some DOB - which I realised utilises 2,5-DMOAmphetamine as a starting material (something I never realised!)
Just curious - as I’ve been looking into making some 3,4,5-trimethoxynitropropene, seeing as I just made the 3,4,5- nitrostyrene.
I’m trying to gather as many as possible so I can do back to back runs of reducing them using the LiAlH4 I have.
Otherwise I will use NaBH4 + CuCl2 instead
I’m thinking far down the line to maybe make some DOB - which I realised utilises 2,5-DMOAmphetamine as a starting material (something I never realised!)
Just curious - as I’ve been looking into making some 3,4,5-trimethoxynitropropene, seeing as I just made the 3,4,5- nitrostyrene.
I’m trying to gather as many as possible so I can do back to back runs of reducing them using the LiAlH4 I have.
Otherwise I will use NaBH4 + CuCl2 instead
no, I'm not a big fan of long acting vasoconstrictors.
If you have both NaBH4 and LiAlH4, I recommend use first one for PEAs and the last one (LAH) for asymmetric Tryptamines like 5-MeO-MiPT, 5-MeO-MET, etc.
If you have both NaBH4 and LiAlH4, I recommend use first one for PEAs and the last one (LAH) for asymmetric Tryptamines like 5-MeO-MiPT, 5-MeO-MET, etc.
Oh really? Okay you have basically told me the opposite of what I was going to do lol
I don’t really plan on exploring many of the 5-meo tryptamine’s, however, iv been performing cold reductive aminations on tryptamine and I know the theory is the same if starting from 5-meo-tryptamine. Surely you don’t mean to use LiAlH4 for that? Boro works great for that purpose.
Do you mean if I were obtaining those 5-Meo tryptamine’s via picktet-Spengler reaction? If that’s even possible with 5-meo tryptamine’s.
You have thrown me a little with that!
I honestly, haven’t even given any 5-MEO tryptamine’s any thought so far!
I have enough on my plate with all these blooming reductions of nitrostyrene’s - I know iv seen people reduce them with NaBH4 and a catalyst - it was CuCl2 for I believe mescaline? Something like that…
I just figured - I have 30g of LiAlH4 and a virtually unlimited supply for NaBH4 as it’s legal here so yeah. I just figured I’d follow Shulgin’s process at least for something.
Its all interesting and I learn something with everything I do! Even if it’s something small like don’t overfill the oil in your vacuum pump or it’ll squirt it through the vent all over the ceiling!! …and me of course!
I don’t really plan on exploring many of the 5-meo tryptamine’s, however, iv been performing cold reductive aminations on tryptamine and I know the theory is the same if starting from 5-meo-tryptamine. Surely you don’t mean to use LiAlH4 for that? Boro works great for that purpose.
Do you mean if I were obtaining those 5-Meo tryptamine’s via picktet-Spengler reaction? If that’s even possible with 5-meo tryptamine’s.
You have thrown me a little with that!
I honestly, haven’t even given any 5-MEO tryptamine’s any thought so far!
I have enough on my plate with all these blooming reductions of nitrostyrene’s - I know iv seen people reduce them with NaBH4 and a catalyst - it was CuCl2 for I believe mescaline? Something like that…
I just figured - I have 30g of LiAlH4 and a virtually unlimited supply for NaBH4 as it’s legal here so yeah. I just figured I’d follow Shulgin’s process at least for something.
Its all interesting and I learn something with everything I do! Even if it’s something small like don’t overfill the oil in your vacuum pump or it’ll squirt it through the vent all over the ceiling!! …and me of course!
NaBH4 for DMT and other substituted DMTs works fine.
I meant asymmetric N,N-methyl,alkyl tryptamines that are accessible via reduction of formyl intermediate to NMT first.
There are different approaches to get desired products though, each with its own pros and cons.
I meant asymmetric N,N-methyl,alkyl tryptamines that are accessible via reduction of formyl intermediate to NMT first.
There are different approaches to get desired products though, each with its own pros and cons.
Yeah that’s what I assumed you meant…well sort of. I certainly assumed you didn’t mean for the easy synthesis iv been following for simple tryptamines!
It’s interesting yeah I didn’t really consider the vasoconstrictor thing to be fair. Yeah I remember having bronco dragonfly and not particularly liking that aspect…
It’s more a case of I have this and this, what different things can I make! I actually rarely consume the psychedelics I make - maybe once every few months and that’s DMT Which lasts like ten mins so yeah I guess your right on that one…
I find it hard to even allot 8 or so hours to an LSD trip. It seems to wear off quicker for me than others but still I do love it.
I think my ultimate goal is 2c-e. Takes a long time to come on and is also a long laster but DAM iv had some great trips on that stuff when all these were easily available from china and Canada.
Having said that - I actually have everything in stock to make 2c-b so that’s my first goal - hence why I was asking about DOB - coz I have bromine lol
It’s interesting yeah I didn’t really consider the vasoconstrictor thing to be fair. Yeah I remember having bronco dragonfly and not particularly liking that aspect…
It’s more a case of I have this and this, what different things can I make! I actually rarely consume the psychedelics I make - maybe once every few months and that’s DMT Which lasts like ten mins so yeah I guess your right on that one…
I find it hard to even allot 8 or so hours to an LSD trip. It seems to wear off quicker for me than others but still I do love it.
I think my ultimate goal is 2c-e. Takes a long time to come on and is also a long laster but DAM iv had some great trips on that stuff when all these were easily available from china and Canada.
Having said that - I actually have everything in stock to make 2c-b so that’s my first goal - hence why I was asking about DOB - coz I have bromine lol
2c-e also does not seem difficult in the end:
You've already learned the Henry reaction, now do the NaBH4+ Cu(II)Cl reduction and all will fall into place.
Oh and there was even some 4-ethyl-2,5-dimethoxynitrostyrene sold on etsy recently albeit a tad pricey. Can't find it now.
You've already learned the Henry reaction, now do the NaBH4+ Cu(II)Cl reduction and all will fall into place.
Oh and there was even some 4-ethyl-2,5-dimethoxynitrostyrene sold on etsy recently albeit a tad pricey. Can't find it now.
- By Rabidreject
Etsy is a mad one like that - my best supplier I found through Etsy. In fact the person that enabled me to do most of this chemistry I met through Etsy.
I just forget to search it regularly - I too have def seen relevant nitrostyrenes on there but as you say was expensive and I figured I needed the practice of getting the aldehyde all the way to the phenethylamine.
Don’t know why - there was just something in me wanting to see these incredible bright coloured needle crystals grow…it really is quite incredible. Especially having come from a reaction that I was having trouble getting to crystallise (DMT).
I just forget to search it regularly - I too have def seen relevant nitrostyrenes on there but as you say was expensive and I figured I needed the practice of getting the aldehyde all the way to the phenethylamine.
Don’t know why - there was just something in me wanting to see these incredible bright coloured needle crystals grow…it really is quite incredible. Especially having come from a reaction that I was having trouble getting to crystallise (DMT).
Better link to 2-e synth: https://www.sciencemadness.org/whisper/viewthread.php?tid=157496&page=3#pid686019
That’s all really useful and interesting…
I actually came back on here because I realised my Benzo detox ravaged brain said the Picktet-Spengler reaction earlier with regards to tryptamine’s and using LAH for that. Brain fart!
I actually meant the reaction whereby tryptamine’s are constructed via indole….mind you I suppose that’s how shulgin gets from tryptamine to things like DMT so I think I get what you mean.
Iv been doing a lot of low temp reductive animations where the Picktet-spengler reaction is a side reaction(hence running at low temps) so sorry about that - although it seems conversation has moved on around my brain farts and typing farts!
I also meant bromo dragonfly earlier!
Yeah see this is essentially why I am intending to turn all the 2,5-DMOBA into the nitrostyrene and then to 2c-h.
That way it can be stored as the salt and basically when I come across the ethylating agent (I can’t say iv read the linked syntheses yet to say what it is - but I will!) and then I can brominate some of it and just store the rest.
Im trying to make the 3,4,5 nitropropene at the mo and going by shulgin’s description of a dark red solution as well as the Mescaline/TMA video on here, mine seems a little too orange - to be honest, iv never done a successful synthesis with this nitroethane (but that doesn’t really mean shit, as iv only tried to use it once before) - i’m at the part where I need to remove the solvent under vacuum (times like these I wish I had a rotovap!)
Guys, I am SO friggin’ close to being free of benzos after twenty odd years - the withdrawal had taken well over a year at this point. I wanted to say sorry as I constantly have a foggy brain and so often make mistakes on here recalling info! Then to add another layer of annoyance it’s all science talk, of which my device’s spell check clearly doesn’t like! Mere weeks left now and I can’t wait….
I must admit chemistry has been a nice distraction and the DMT and other simple tryptamine’s it has so far provided have certainly helped!
It’s going to be interesting when I restart my BA Hons in art, whilst also studying degree level chemistry books in my spare time haha bit of a mad mix to be fair! Life is…interesting
I actually came back on here because I realised my Benzo detox ravaged brain said the Picktet-Spengler reaction earlier with regards to tryptamine’s and using LAH for that. Brain fart!
I actually meant the reaction whereby tryptamine’s are constructed via indole….mind you I suppose that’s how shulgin gets from tryptamine to things like DMT so I think I get what you mean.
Iv been doing a lot of low temp reductive animations where the Picktet-spengler reaction is a side reaction(hence running at low temps) so sorry about that - although it seems conversation has moved on around my brain farts and typing farts!
I also meant bromo dragonfly earlier!
Yeah see this is essentially why I am intending to turn all the 2,5-DMOBA into the nitrostyrene and then to 2c-h.
That way it can be stored as the salt and basically when I come across the ethylating agent (I can’t say iv read the linked syntheses yet to say what it is - but I will!) and then I can brominate some of it and just store the rest.
Im trying to make the 3,4,5 nitropropene at the mo and going by shulgin’s description of a dark red solution as well as the Mescaline/TMA video on here, mine seems a little too orange - to be honest, iv never done a successful synthesis with this nitroethane (but that doesn’t really mean shit, as iv only tried to use it once before) - i’m at the part where I need to remove the solvent under vacuum (times like these I wish I had a rotovap!)
Guys, I am SO friggin’ close to being free of benzos after twenty odd years - the withdrawal had taken well over a year at this point. I wanted to say sorry as I constantly have a foggy brain and so often make mistakes on here recalling info! Then to add another layer of annoyance it’s all science talk, of which my device’s spell check clearly doesn’t like! Mere weeks left now and I can’t wait….
I must admit chemistry has been a nice distraction and the DMT and other simple tryptamine’s it has so far provided have certainly helped!
It’s going to be interesting when I restart my BA Hons in art, whilst also studying degree level chemistry books in my spare time haha bit of a mad mix to be fair! Life is…interesting