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.
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.
