The simplest recipe for crystal Mephedrone
- Thread starter Madre
- Start date
I just make it once, I make methylene solution myself, I used cold distilled water for it, then I add it to 2b4mp with benzene, somehow I already can see the separation of layers, anyone can help me ? Because I wash it with water on next step, eventually the outcome is so little, I’m afraid the product was left in the water layer, instead of the top organic layer
- By 61-50-7
If it's really methylene and not a typing error then you'll never get product from it; you need to add methylamine to the solution and that's only when the reaction is complete that meph is dissolved into benzene, 2B4M is polar so soluble in water, thats where reaction happens
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- By WalterFan
Sorry, it is type error, what I have is cas 593-51-1; after read your opinion, can i basically only use water to dissolve cas 1451-82-7, then adding NaOH in water, mixed it together first, then slowly adding MA.HCI into the RM and stir, the whole process should be under 30 Celsius and sealed. After all, I finally added benzene for extraction and acidify the benzene layer. Would it be the same, or you have any advice of this idea ? Because I only had few grams product from the benzene layer last time, I strongly believe most of the unreacted Cas 1451 was still left in the water layer, I desperately don’t know how to fix it yesterday.
- By 61-50-7
Ethyl acetate is preferrer and you can add MeNH2 quickly (with etoac), here a good topic for thhat https://bbgate.com/en/threads/mephe...hyl-acetate-methylamine-hcl.12336/#post-68474
I have a bunch of questions that I hope someone can answer for me.
1. Solvent
Benzene is hard to obtain in the EU and after discussing this synthesis I've decided to use DCM instead. The original recipe uses 200 ml of benzene but it seems that when DCM is used, 500 ml is a popular amount for the same amount of 2b4mp. How does the different amount of solvent affect the process? Besides better thermal stability during amination (more solvent = more RM volume = it does not heat up as much as compared to lower volume of RM), does the use of more solvent have any other benefits? And can the 500 ml of DCM be cut down to say a half, i.e. 250 ml? (I am aware of the low boiling point of DCM and the necessity to keep the RM below 40 °C.)
2. Methylamine (MA)
MA hydrochloride (MA.HCl) seems to be a popular alternative to aqueous MA (easier transport, storage, stability). Can you just add a base into the RM together with 2b4mp and solvent, and then add MA.HCl directly into the RM? I am advised to use triethylamine as base, would NaOH work equally well?
3. Acidification
This recipe instructs to create a mix of HCl in acetone and add this mixture into the RM in small portions. In other tutorials acetone is added first and HCl is then added drop-wise. Which way is better and why?
4. Filtration
This being the simplest recipe, vacuum filtration using Schott/Buchner funnel is not available. Can I use coffee filters and gravity filtration instead?
5. Acetone
My acetone is declared >99.6 % pure, water content is not declared by the producer. Is my acetone considered dry for this application?
6. Personal protective equipment
Is a gas mask required, or can one wing this with good ventilation or by working in open air?
7. Waste management
I see three types of waste:
1. Solvent
Benzene is hard to obtain in the EU and after discussing this synthesis I've decided to use DCM instead. The original recipe uses 200 ml of benzene but it seems that when DCM is used, 500 ml is a popular amount for the same amount of 2b4mp. How does the different amount of solvent affect the process? Besides better thermal stability during amination (more solvent = more RM volume = it does not heat up as much as compared to lower volume of RM), does the use of more solvent have any other benefits? And can the 500 ml of DCM be cut down to say a half, i.e. 250 ml? (I am aware of the low boiling point of DCM and the necessity to keep the RM below 40 °C.)
2. Methylamine (MA)
MA hydrochloride (MA.HCl) seems to be a popular alternative to aqueous MA (easier transport, storage, stability). Can you just add a base into the RM together with 2b4mp and solvent, and then add MA.HCl directly into the RM? I am advised to use triethylamine as base, would NaOH work equally well?
3. Acidification
This recipe instructs to create a mix of HCl in acetone and add this mixture into the RM in small portions. In other tutorials acetone is added first and HCl is then added drop-wise. Which way is better and why?
4. Filtration
This being the simplest recipe, vacuum filtration using Schott/Buchner funnel is not available. Can I use coffee filters and gravity filtration instead?
5. Acetone
My acetone is declared >99.6 % pure, water content is not declared by the producer. Is my acetone considered dry for this application?
6. Personal protective equipment
Is a gas mask required, or can one wing this with good ventilation or by working in open air?
7. Waste management
I see three types of waste:
- the aqueous fraction discarded during free base flushing in step 2. This should be just water with some Bromine in it, is it safe to discard in a residential location?
- the solvents (DCM and acetone) separated during filtration in step 4 and acetone used for washing. How do you discard it safely and responsibly while avoiding cursory screening by the water treatment company?
- used indicator paper, used filter paper and similar waste material. I assume this can be wrapped, sealed and discarded with household waste, am I right?
- By Dr. MMX
glad to hear your doing your 1st steps into that
i simply recommend my method thats posted in synthesis section. I believe I asked you a question if u wanna go easy one or teaching one. Simply choice ethyl acetate and use it for your synthesis. You can use DCM as well but i dont recomment it as 1st stynthesis. You will need more eqfor DCM. In DCM general ruleis that you cant get over 38c becasue it will boil, simply keep temperature at 36-37c and you will have its reaction on about 3h, sometimes less sometimes more. You will know its end of reaction once temperature will not keep itself (abit)
2. You can use HCL methylamine + NaOh, you can use 40% aq solution, you can do 40% aq solution urself(best method). But to do it urself you need serious exhaust fan and a bnit more serious conditions.
3. always one drop per 1s, you can go faster if you know what ur doing, but for start go that way.
4. You can use gravity filtration you can use even cloth for it, its all ok. Buchner/vacuum just helps and makes it faster.
5. 99.6% is good acetone
6. Mask is absolutely required, maybe someone experienced withvery goodexhaust could decide to not wear mask in small scale. For u its necesarry, gloves as well
7. solid wastes put into one bag and throw it to bin far from home, liquids canbe distilled to recover them, but otherwise just spill it in some soil outside when nobody sees.
i simply recommend my method thats posted in synthesis section. I believe I asked you a question if u wanna go easy one or teaching one. Simply choice ethyl acetate and use it for your synthesis. You can use DCM as well but i dont recomment it as 1st stynthesis. You will need more eqfor DCM. In DCM general ruleis that you cant get over 38c becasue it will boil, simply keep temperature at 36-37c and you will have its reaction on about 3h, sometimes less sometimes more. You will know its end of reaction once temperature will not keep itself (abit)
2. You can use HCL methylamine + NaOh, you can use 40% aq solution, you can do 40% aq solution urself(best method). But to do it urself you need serious exhaust fan and a bnit more serious conditions.
3. always one drop per 1s, you can go faster if you know what ur doing, but for start go that way.
4. You can use gravity filtration you can use even cloth for it, its all ok. Buchner/vacuum just helps and makes it faster.
5. 99.6% is good acetone
6. Mask is absolutely required, maybe someone experienced withvery goodexhaust could decide to not wear mask in small scale. For u its necesarry, gloves as well
7. solid wastes put into one bag and throw it to bin far from home, liquids canbe distilled to recover them, but otherwise just spill it in some soil outside when nobody sees.
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Thank you for the answers! Few more points to clarify, if you don't mind:
3. Is it better to first add all acetone (e.g. 400 ml) and then add HCl 1 drop/s, or first mix 40 ml of HCl in 400 ml of acetone and then add this mixture slowly in small portions?
7. I don't think spilling solvents like EA or acetone is a good idea. Would it be possible to just let them evaporate, boil off or even burn in fire (spray small amounts from a syringe into camp fire)?
3. Is it better to first add all acetone (e.g. 400 ml) and then add HCl 1 drop/s, or first mix 40 ml of HCl in 400 ml of acetone and then add this mixture slowly in small portions?
7. I don't think spilling solvents like EA or acetone is a good idea. Would it be possible to just let them evaporate, boil off or even burn in fire (spray small amounts from a syringe into camp fire)?
May I have a question about the ma.HCI part ? I’ve watched your other post about adding ma.HCI directly into the mixture, and I also try it once recently, I have a problem when I dissolved the 2b4m in solvent, should I followed with NaOH + water and start stirring, then adding MA.HCI immediately with small portions? If I didn’t misunderstand it, the whole mixture would turn dark after adding NaOH water, it’s happening before any MA.HCI followed, because it was what happened during my synthesis, so am I did anything wrong ? Or it is normal ? Best regards
May I have a question about the ma.HCI part ? I’ve watched your other post about adding ma.HCI directly into the mixture, and I also try it once recently, I have a problem when I dissolved the 2b4m in solvent, should I followed with NaOH + water and start stirring, then adding MA.HCI immediately with small portions? If I didn’t misunderstand it, the whole mixture would turn dark after adding NaOH water, it’s happening before any MA.HCI followed, because it was what happened during my synthesis, so am I did anything wrong ? Or it is normal ? Best regards
- By 61-50-7
Hi, I never try with ma HCl personnally but water turning black with naoh is not very surprising, try to add rge ma hcl not too slow tho, just avoid overheating. sorry for the late reply, I didn't logged for a while. try reX in ipa if the product gets dirty
Hi new to this stuff, my synthesis calls for Methylamine free base 40% in (aqueous solution) where would I obtained this without having to go through the trouble of ordering from a big chemical supplier? Thank you