First time 4mmc synth assistance

[dodobird]

For the initial demo run to show the contracting party i plan to use
2b4m 250 gms dissove it in Ethyl acetate 1000 ml in a 3 neck flask, keeping temp below 60 deg with a cold water bath. Add 500 ml of aq ma 40% in 2 or 3 parts while shaking/stirring. Either shake manually or might use a mag stirrer if available. From what i read, i might need to gently heat to about 40-45 deg c to achieve the desired color of crude 4mmc in Ea(should it be dark yellow or brown?). Leave alone for 2 hours.
Once visible freebase layer visibly forms and separates, drain ea ma layer which should be at the bottom.
Add 1000 ml of naco3 plus distilled water and wash the freebase once after stir/shake/swirl ( does the flask need to be sealed or open here).
Wash 2x or 3x with d water until no fishy or ma smell.
Add 500 ml chilled dry acetone (is this regular acetone), stirring while doing this.
Add chilled hcl 38 drop wise until litmus shows exactly between the yellow and orange. (Please let me know which exact color shows ph5.5?).
Stir a couple of minutes, take off and cover this beaker using a cling wrap or sanwich plastic. Place at about 10dg for an hour then in freezer 1dg for an hour or two.
Filter this with cold acetone until almost white salt remains . Leave pump on for 20 minutes so all liquid drained.
Recrystallize using 30ipa 70h20 solution in parts.
Appreciate any remarks feedback shortcuts corrections and guidance to enable this humble first timer to nail it nicely and chalk one up for the bbgorum.

I have the procedure set in my mind but a step by step here using minimal lab eq and no extra reagents would be bolstering ny self belief.
I want to synthesize quality and potent 4mmc withing the shortest time period.

Thanks in advance.

 

[Berlin777]

Why cold water bath if you dissolving 2b4mp?

 

[dodobird]

Sorry bout that you're right my text edit was incorrect. Add ea n heat no bath here but next step with ma

 

[William D.]

Tell us where you read this method?

 

[dodobird]

I've gathered this from various posts.. appreciate constructive criticism if you would be so kind

 

[William D.]

(click) - this is not the best synthesis, but you see better in the video. This is easier than you think.
(click) - here you can see in more detail on other equipment

 

[dodobird]

The Voss method was my first choice but couldn't get 4mp
Please point out the flaws in mybtheoretical method above. Would be eternally obliged

Are the measurements off and if so for which part.
Am I doing something really wrong there

 

[dodobird]

Wit the reagents I have n all.. whats the easiest way to synth from 250 gms 2b4m using ea ma 40 and acetone and hcl38?

 

[dodobird]

Anyone?????

 

[dnBQByvHb8Zkawbjpx]

It looks like you have the process and all steps of the synthesis researched thoroughly. Here's my few notes:

• 500 ml acetone is too little for 250 g 2b4m. Have at least a liter, better 1.5 liters, available in your freezer. You may not need to use all but with 500 ml you would be rather short. Acetone used at this step can be recovered and reused again after a distillation.
• a magnetic stirrer/hot plate is an absolute must for consistency. It's the best $100 spent towards making 4-MMC .
• "drain ea ma layer which should be at the bottom" EA stays on top (it contains your free base), water that came from the MA aq 40 % is at the bottom. Drain water, like in all future washing steps.
• "does the flask need to be sealed or open here" always sealed, you can vent to release any pressure once done shaking
• your magnetic stirrer will not be able to work properly once the mixture thickens due to precipitated 4-MMC.HCl. Plan for this moment and have at least a spatula waiting, if not an overhead stirrer.
• dry acetone is acetone with as little water as possible. You should distill store-bought acetone to remove any contained water and impurities, but acetone purchased from trusted lab chemicals suppliers that is >99.5 % pure will work ok as well
• recrystallization does not require any other solvents than water, other solvents may speed up the process a little but they're costly so try and see how pure distilled water works for you. After some attempts with IPA and ethanol I don't use anything else anymore
• don't start with large (100 g or more) batches. Scale down the standard recipe to 1/4 and start with 25 g of BK4. That way you can confirm the process and everything works as you expect without wasting precious reagents before you get everything right. Once you confirm all is fine you scale up to 100 g batches or larger.

Hope this helps, good luck!