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William Dampier

Well-known member
Expert
Joined
Jul 19, 2021
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384
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Reaction scheme:
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Reagents:
1. 4'-Methylpropiophenone (cas 5337-93-9) 1 kg;
2. Hydrobromic acid 48% 960 ml;
3. Hydrogen peroxide 35% 636 ml;
4. Sodium/potassium hydroxide 25% (NaOH/KOH) aqueous solution;
5. Distilled water;
6. Ethyl acetate 6 l;
7. Methylamine 40% aq - 2 l;
8. Acetone - 8 l;
9. Hydrochloric acid (HCl 38%) 500 ml;
10. Isopropyl alcohol;


Equipment and glassware:
1. Scales;
2. Jacketed 10 L reactor equipped with reflux condenser, drip funnel, thermometer, top stirrer and temperature control system;
3. Heating pump;
3. Chiller pump;
4. Vacuum source;
5. Buckets;
6. Freezer;
7. Pyrex dishes;
8. Nutsche filter;
9. pH indicator papers;


Stage 1. Halogenation.
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1. 4'-Methylpropiophenone (cas 5337-93-9) 1 kg is weighted and poured into a 10 L reactor;
2. Hydrobromic acid (HBr 48%) 320 ml is added and stirred for 5 min.
3. Hydrogen Peroxide (H2O2 35% 212 ml) is poured into a drip funnel and installed onto the reactor neck.
4. Drip funnel tap is opened and hydrogen peroxide is added dropwise with a constant stirring.
5. Color of the mixture may vary from yellow to red. Hydrogen peroxide is added in order to discolor the mixture.
6. Temperature is kept up to 65 °C. If reaction temperature is higher, hydrogen peroxide addition is stopped.
7. Step 2-6 are repeated twice after hydrogen peroxide addition.
8. Crystallization can start during the reaction. Hydrobromic acid and hydrogen peroxide are added dropwise until the end of amount and stirred for 1.5-12 h.
9. Next, distilled water is added and stirred for 5 min.
10. Stirring is stopped. Reaction mixture is left until entire 2-bromo-4'-methylpropiophenone is fallen down in the reactor.
11. Water is removed with help of pump through the reactor neck.
12. Sodium/potassium hydroxide 25% (NaOH/KOH) aqueous solution is added to the reaction solution and stirred for 5 min.
13. Repeat 9, 10, 11 steps.
14. The resulting product is left in the reactor.

Stage 2. Methamination.
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1. Ethyl acetate 6 l is poured into the reactor.
2. Reaction mixture is stirred and heated in Jacketed reactor up to 30 °C with help of heating system.
3. The mixture is stirred until complete amount of 2-bromo-4'-methylpropiophenone (cas 1451-82-7) is dissolved.
4. The stirring is stopped. The reaction mixture is left for layer separations. A bottom layer is drained through a bottom reactor tap.
5. The stirrer is turned on and methylamine 40% aq 2 l is added at once.
6. The mixture is stirred for 20 min, temperature is kept below 65 °C.
7. Repeat step 4.
8. After that, the mixture is heated up to 65 °C and reactor vacuum pump is turned on. The reactor condenser chiller pump is turned on as well.
9. All amount of ethyl acetate or the biggest part of it is distilled off.
10. Vacuum pump is turned off. Acetone is added to the reactor with a constant stirring.
11. Hydrochloric acid (500 ml) is placed into the drip funnel and the funnel is installed onto the reactor neck.
12. Hydrochloric acid is added dropwise to reach pH 5 with constant stirring. A small amount (~2-5 ml) of reaction mixture is drained from the bottom reactor tap in order to check pH by pH indicator stripe. The sample is poured back into the reaction mixture.
13. After that, the mixture is poured into a bucket and the bucket is put into a freezer for 12 h.


Stage 3. Filtration.
1. A vacuum filtration system (Nutsche filter, filter cloth, vacuum pump) is assembled and installed.
2. The vacuum pump is turned on.
3. A bucket content from step 13 stage 2 is poured to the
Nutsche filter.
4. The mixture is filtered and pressed until the funnel content is become solid.
5. A cold dry acetone is poured onto the solid product in the funnel in several small portions during filtration.
6. Acetone is filtered. Step 5 is repeated, if the solid is not white.
7. White solid 4-MMC product is moved into a Pyrex dish for a drying after filtration procedure.
8. Pyrex dish with 4-MMC is placed into a dry well ventilated warm room.
9. 4-MMC product is dried to a constant mass. Product is mixed and grinded periodically in order to increase drying speed.


Stage 4. Recrystallisation.

Mephedrone (4MMC) crystallization
 
Last edited by a moderator:

woohoo

Member
Joined
Apr 21, 2022
Messages
54
Reaction score
13
Points
8
Didn't it should be separated from n-methylacetamide?
Seems its dirty reaction, how much it yields in comparison with nmp or aromatic solvent?
 
Joined
May 18, 2022
Messages
56
Reaction score
17
Points
8
N-methylacetamide should be soluble in acetone, though I could not find how much. Freebase is indeed black and resulting powder turns green upon addition of crystalizing solvent mix (unreacted ketone?). Its safe to assume this isn't the cleanest procedure.

Some swear that any other reaction besides one using NMP as a solvent produces much, much inferior results in final product. More of the speedy high without any euphoria.

Did you run GC-MS to see if there are any impurities in resulting powder/ crystals?
@G.Patton
@Marvin "Popcorn" Sutton
@William Dampier
 

G.Patton

Well-known member
Expert
Joined
Jul 5, 2021
Messages
1,257
Reaction score
755
Points
113
Freebase is indeed black and resulting powder turns green upon addition of crystalizing solvent mix (unreacted ketone?). Its safe to assume this isn't the cleanest procedure.
Hi, probably you did something wrong or your reagents not so good. Yes, we did GC-MS. 96.4% 4-MMC
PwIN6e4125
 

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Joined
May 18, 2022
Messages
56
Reaction score
17
Points
8
I didn't try this reaction yet. I watched video published here iodo-ketone amination. There I saw freebase is black and powder changed colour when preparing for crystalization. Maybe it was black cause of iodine being leaving group as opposed to bromine.
Questions to comfirm:

1. Results above are from ethyl acetate as a solvent ?
2. Have you done this reaction with EA and bromoketone, does freebase look any different?
3. I noticed from video that crystals from EA look glass like, while NMP are lot whiter. I read your post about stereochemistry of 4-MMC how S and R enantiomers form different looking crystals, are both of these crystals equally racemic?
4. Did you notice any difference in subjective effect between EA and say NMP in final product?

Thank you for posting these results.
 

G.Patton

Well-known member
Expert
Joined
Jul 5, 2021
Messages
1,257
Reaction score
755
Points
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1. Results above are from ethyl acetate as a solvent ?
Actually I don't remember for sure. Probably yes.
3. I noticed from video that crystals from EA look glass like, while NMP are lot whiter. I read your post about stereochemistry of 4-MMC how S and R enantiomers form different looking crystals, are both of these crystals equally racemic?
Yes, these are racemic crystals.
4. Did you notice any difference in subjective effect between EA and say NMP in final product?
I haven't tasted the product as any good wine manufacturer =)
 
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