Ok, did I understand this correctly?
Step 1: Two solutions are prepared:
Solution 1: 100 g of 2b4m are dissolved in 500 mL of DCM
Solution 2: 200 mL of a 40% methylamine solution
Both solutions are combined in a container, which is then sealed and shaken for 30 minutes.
Step 2: Approximately 200 mL of water is added to the mixture and shaken.
The aqueous phase is discarded. This step is repeated 2-3 times.
The lower phase now consists of DCM and 4-mmc freebase.
Step 3: A solution is prepared consisting of 55 mL of HCL and 500 mL of acetone.
This solution is added to the dcm/4-mmc mixture until the pH level reaches 5.5-6.0.
Step 4: The solution is evaporated until the 4-mmc precipitates out as a salt.
Step 1: Two solutions are prepared:
Solution 1: 100 g of 2b4m are dissolved in 500 mL of DCM
Solution 2: 200 mL of a 40% methylamine solution
Both solutions are combined in a container, which is then sealed and shaken for 30 minutes.
Step 2: Approximately 200 mL of water is added to the mixture and shaken.
The aqueous phase is discarded. This step is repeated 2-3 times.
The lower phase now consists of DCM and 4-mmc freebase.
Step 3: A solution is prepared consisting of 55 mL of HCL and 500 mL of acetone.
This solution is added to the dcm/4-mmc mixture until the pH level reaches 5.5-6.0.
Step 4: The solution is evaporated until the 4-mmc precipitates out as a salt.
- By HerrHaber
the hydrochloride should precipitate upon acidification, and partial evaporation is inevitable but I'm not 100% sure you should waste your time trying to evaporate (rather concentrate) the suspension, instead place it in the freezer for some hours and then filter it, you are advised to let the filtrate (remaining liquid) evaporate some more then freeze again for a second crop of lesser quality (considering everyone wants to see them big crystals recrystalization is a must, you can combine the solids or recryst separately if the second one has an obvious drop in quality)
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- By HerrHaber
Good question! For amphetamine i used 1:10 dilution of H2SO4 in acetone and more acetone added to the freebase solution to achieve good results (the acid acetone mix should always be discarded after use best is to first clean something really dirty and hydrophobic). In the case of cathinones I add quite more freezer cold acetone to the freebase and add the conc. acid dropwise with much care and pH paper (there were times when as soon as pH was decreasing towards neutral I added 1-3 times the volume of acid worth of acetone over it in the dropping funnel and then give it a swirl (note that this is a.q. HCl 37%) the large volume ratio of acetone to acid make's the water brought with the acid to be less likely to dissolve your product. Also keep a considerable amount for 3 to 5 washes on the filter paper not to have to do repeated recrystalizations (prepare for at least two if material isn't white after washing) and also let it cool down to freezer temperature before and after adding the acid (including the acid), you may also generate hydrogen chloride gas if the batch is considerable (i never add the whole 55 mL's of HCl not to let the pH too low) but my yields weren't as good as presented until recently when I found out the flaw and the way to correct it. Also my NMP is on the way, I worked with AcOEt, DMF and DCM they all work but I know now to approach the workup in slightly different way as suitable for the solvent (less water for the acetate and much more for DMF followed by the extraction of the a.q. phase with 2 x not much DCM). As I said you are not doing it wrong even I do it in a similar fashion, though, acetone freezer temp. before the acid also freezer temp make's more sense as well as diluting your acid with acetone as you are getting close to neutral not to add an excess by accident.
- By SonicNL
Thanks alot for your detailed reply.
However, this only raises more questions. The saying the more you know, the less you understand goes up I guess.
Lets jump on-topic.
What makes the product dissolve? And this is useful advice.
What was the flaw?
So it would make more sense to make a solution acetone / HCI, and store it on freezer temp before acidifying. I'm going to try this.
Well, when I spoke to another respected member on this forum, and he said doing it my way was wrong. Yours is right.
But I want to know why, just copying other peoples methods may work, but i'm trying to understand why it works. Lol.
I also have a question regarding the ideal temp on DCM.
Currently i'm heating to 37 C half an hour after adding methylamine, and let the solution stir for 4 hours.
Have you, or any other contributors on this forum advice on the ideal heating temperature and time for methylamation on DCM, 1:5 ratio with ketone?
However, this only raises more questions. The saying the more you know, the less you understand goes up I guess.
Lets jump on-topic.
What makes the product dissolve? And this is useful advice.
What was the flaw?
So it would make more sense to make a solution acetone / HCI, and store it on freezer temp before acidifying. I'm going to try this.
Well, when I spoke to another respected member on this forum, and he said doing it my way was wrong. Yours is right.
But I want to know why, just copying other peoples methods may work, but i'm trying to understand why it works. Lol.
I also have a question regarding the ideal temp on DCM.
Currently i'm heating to 37 C half an hour after adding methylamine, and let the solution stir for 4 hours.
Have you, or any other contributors on this forum advice on the ideal heating temperature and time for methylamation on DCM, 1:5 ratio with ketone?
- By mocnykutas
you can add all the methylamine at once it's nonsense you don't have to add it for an hour xD
