BMK methyl glycidate
Cas no: 80533-66-7
P2P phenylacetone phenyl-2+propanone
Cas no: 103-79-7
Prep for stage 2:
1. Dissolve .5 KG of methylamine per 5 L of methanol.
2. Dissolve .310 KG of sodium hydroxide in 5 L of methanol.
3. Slowly add the lye mix in methylamine mix while keeping chiller set to 0c and stirring thoroughly.
Starting From BMK
Stage 1 in 100 L jacketed reactor
Hydrolysis of BMK glycidate and then Decarboxylation to P2P
1: add 1 KG of BMK into 5 L of HCL, stir and heat to 100c for 2 hours or until all BMK dissolved/turns to oil
2. Add a lye solution while cooling until reach 10.5 PH.
3. Settle mixture and separate.
4. Add 2 L of DCM to bottom materiel and mix.
5. Let bottom mix settle, drain DCM and rotovap at 50 C
6. Mix roto'd bottom mix with top mix and stir, this is now P2P
Stage 2 in 100 L double jacketed reactor
If have P2P can start at this stage
Reductive Amination
1. Add 2 L of methanol to Reactor.
2. Add 1 KG of P2P and stir .
3. Set Reactor to -0c Slowly add prep 2 mix (approx 10 L)
4. Add 40 grams of lye and stir for 20 minutes.
5. When temperature gets to 0c-5c start to slowly add 127 grams of sodium borohydride (per KG of P2P oil) (in small increments of 5-10 grams). Do not let go above 25c
6. Stir for 3 hours at room temp.
7. Rotovap everything at 50 C.
Stage 3.
1. Add 5 L of water per 1 KG of stage 2.
2. Add 2 L of DCM stir for 15 minutes at room temp .
3. Stop stirring and settle and drain DCM into buckets.
4. Repeat step 2 and 3.
5. Repeat step 2 and 3.
6. Scrap remaining waste in reactor.
7. Add all DCM pulls back into reactor.
8. Add 1:1 water and HCL mix into cone slowly while keeping below 25 C until reach PH of 1.5. Then stop stirring and let settle.
9. Separate top and bottom mix and drain into buckets.
10. Re add bottom mix to reactor and add 5 L of water and stir for 15 minutes. Then let settle.
11. Separate top and bottom layers, re add bottom mix to reactor and repeat step 10.
12. Scrap bottom mix and add all top mixes back into reactor.
13. Add lye solution until PH 10.5
14. Add 5 L of DCM stir and then settle and pull DCM into buckets. Repeat this 2 more times. Everything left in reactor is now waste. Rotovap all DCM out of buckets at 50 C.
Stage 4
1. Add 1 litre of cold acetone and 1 KG of finished stage 3 into 100 L Reactor.
2. Set reactor to -0 and slow drip 37%HCL acid until reach a PH of 2 .
3. Drain reactor into buckets half full of -20 acetone to crash crystal/pow and put in freezer for 24 hours.
4. Buchner the powder crystal, and keep the liquid and reheat and evaporate out 40% of volume and then re acidify until 2 PH and crash again into -20 Ace and then in freezer for another 24 hours to try and reclaim any missed yield.
Stage 5
1. Dissolve crystal/pow in 80C water/IPA.
2. Pour so 4.5 inches deep in sharding trays.
3. Let recrystallize into shards for a few days and then harvest.
4. Heat liquid until 80c again repeat steps 2 , 3 and 4 until no more crystalization occurs.
Cas no: 80533-66-7
P2P phenylacetone phenyl-2+propanone
Cas no: 103-79-7
Prep for stage 2:
1. Dissolve .5 KG of methylamine per 5 L of methanol.
2. Dissolve .310 KG of sodium hydroxide in 5 L of methanol.
3. Slowly add the lye mix in methylamine mix while keeping chiller set to 0c and stirring thoroughly.
Starting From BMK
Stage 1 in 100 L jacketed reactor
Hydrolysis of BMK glycidate and then Decarboxylation to P2P
1: add 1 KG of BMK into 5 L of HCL, stir and heat to 100c for 2 hours or until all BMK dissolved/turns to oil
2. Add a lye solution while cooling until reach 10.5 PH.
3. Settle mixture and separate.
4. Add 2 L of DCM to bottom materiel and mix.
5. Let bottom mix settle, drain DCM and rotovap at 50 C
6. Mix roto'd bottom mix with top mix and stir, this is now P2P
Stage 2 in 100 L double jacketed reactor
If have P2P can start at this stage
Reductive Amination
1. Add 2 L of methanol to Reactor.
2. Add 1 KG of P2P and stir .
3. Set Reactor to -0c Slowly add prep 2 mix (approx 10 L)
4. Add 40 grams of lye and stir for 20 minutes.
5. When temperature gets to 0c-5c start to slowly add 127 grams of sodium borohydride (per KG of P2P oil) (in small increments of 5-10 grams). Do not let go above 25c
6. Stir for 3 hours at room temp.
7. Rotovap everything at 50 C.
Stage 3.
1. Add 5 L of water per 1 KG of stage 2.
2. Add 2 L of DCM stir for 15 minutes at room temp .
3. Stop stirring and settle and drain DCM into buckets.
4. Repeat step 2 and 3.
5. Repeat step 2 and 3.
6. Scrap remaining waste in reactor.
7. Add all DCM pulls back into reactor.
8. Add 1:1 water and HCL mix into cone slowly while keeping below 25 C until reach PH of 1.5. Then stop stirring and let settle.
9. Separate top and bottom mix and drain into buckets.
10. Re add bottom mix to reactor and add 5 L of water and stir for 15 minutes. Then let settle.
11. Separate top and bottom layers, re add bottom mix to reactor and repeat step 10.
12. Scrap bottom mix and add all top mixes back into reactor.
13. Add lye solution until PH 10.5
14. Add 5 L of DCM stir and then settle and pull DCM into buckets. Repeat this 2 more times. Everything left in reactor is now waste. Rotovap all DCM out of buckets at 50 C.
Stage 4
1. Add 1 litre of cold acetone and 1 KG of finished stage 3 into 100 L Reactor.
2. Set reactor to -0 and slow drip 37%HCL acid until reach a PH of 2 .
3. Drain reactor into buckets half full of -20 acetone to crash crystal/pow and put in freezer for 24 hours.
4. Buchner the powder crystal, and keep the liquid and reheat and evaporate out 40% of volume and then re acidify until 2 PH and crash again into -20 Ace and then in freezer for another 24 hours to try and reclaim any missed yield.
Stage 5
1. Dissolve crystal/pow in 80C water/IPA.
2. Pour so 4.5 inches deep in sharding trays.
3. Let recrystallize into shards for a few days and then harvest.
4. Heat liquid until 80c again repeat steps 2 , 3 and 4 until no more crystalization occurs.
I've never tried or even looked at this reaction, but I see something that chemically dont make sense to me, but Im no a chemist, i just play one on the dark web. you are crystallizing at ph 2. This shit will rot your teeth out in a week. I've never in my life heard of acidifying a drug to 1.5. Theres not a scenario ive ever seen that called for that