Big thanks to @William Dampier and @Marvin "Popcorn" Sutton who did incredible job on mentoring me without whom this wouldn't be possible.
1. Bromo-ketone was looking dirty from remaining bromine. It was washed 3 times with 10% NaHCO3 solution to make water soluble bromine salts hence removing the orange color. If manual stirrer is not available, best way l find is to brake up large chunks with spatula and shake vigorously. It's important to went frequently to avoid pressure build up from CO2.
2. Cleaned bromo-ketone (still wet from previous step) was mixed with 200 ml of DCM and put under strong stirring. Quickly, everything dissolved and ~25 ml of MeNH2 was added. Slight exothermic reaction happen, but not extreme so the rest of amine was added. For the first hour RM was self-heated and stirred. For the remaining two, heating was applied and the temperature kept at ~35 degrees celsius.
3. After 3 hours the RM color got more pronounced. 100ml of water was added and RM was transfered to separatory funnel. Layers were allowed to separate and upper aqueous removed. Water washing procedure was repeated as long as there was amine smell present. In this case two.
4. I decided to dry things up with MgSO4.
5. Filter the freebase.
5. Add HCl directly to freebase, diluted with acetone. I find It's important to take time and acidify slowly. Luckily, l managed to be spot on. pH was 6.
6. Salt was filtered and washed with acetone 3x times.
My yield was 50% which is on the lower side. I thing it's mostly due to my sloppiness- one major spill, which happen unfortunately. Last time l had lab work was over a year ago. Nevertheless, l did what l made with some friends and it's mix of coke and mdma on rocket fuel. So l call this success =)
Pictures are in order chronologically.
1. Bromo-ketone was looking dirty from remaining bromine. It was washed 3 times with 10% NaHCO3 solution to make water soluble bromine salts hence removing the orange color. If manual stirrer is not available, best way l find is to brake up large chunks with spatula and shake vigorously. It's important to went frequently to avoid pressure build up from CO2.
2. Cleaned bromo-ketone (still wet from previous step) was mixed with 200 ml of DCM and put under strong stirring. Quickly, everything dissolved and ~25 ml of MeNH2 was added. Slight exothermic reaction happen, but not extreme so the rest of amine was added. For the first hour RM was self-heated and stirred. For the remaining two, heating was applied and the temperature kept at ~35 degrees celsius.
3. After 3 hours the RM color got more pronounced. 100ml of water was added and RM was transfered to separatory funnel. Layers were allowed to separate and upper aqueous removed. Water washing procedure was repeated as long as there was amine smell present. In this case two.
4. I decided to dry things up with MgSO4.
5. Filter the freebase.
5. Add HCl directly to freebase, diluted with acetone. I find It's important to take time and acidify slowly. Luckily, l managed to be spot on. pH was 6.
6. Salt was filtered and washed with acetone 3x times.
My yield was 50% which is on the lower side. I thing it's mostly due to my sloppiness- one major spill, which happen unfortunately. Last time l had lab work was over a year ago. Nevertheless, l did what l made with some friends and it's mix of coke and mdma on rocket fuel. So l call this success =)
Pictures are in order chronologically.
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