Introduction
This theme is dedicated to syntheses of 3-Fluoromethcathinone (3-FMC; CAS 1346600-40-5) and 3-Chloromethcathinone (3-CMC; CAS 1607439-32-6) precursors as well as their ortho-analogues (2-FMC and 2-CMC) 3'-Chloropropiophenone CAS 34841-35-5 and 3'-Fluoropropiophenone CAS 455-67-4.
2-CMC, 3-CMC and and fluoro-analogues are quite popular in Western Europe and these rather simple methods allow clandestine chemists to produce precursors for these methcathinones by yourself.
2-CMC, 3-CMC and and fluoro-analogues are quite popular in Western Europe and these rather simple methods allow clandestine chemists to produce precursors for these methcathinones by yourself.
Difficulty rating: 4/10
3'-Chloropropiophenone CAS 34841-35-5
- 10 L three-necked round bottom flask
- Reflux condenser;
- Funnel;
- Distillation apparatus;
- Rotory evaporator;
- Vacuum pump;
- Buchner flask and funnel (large);
- Beakers 5L; 2l x2
- Measuring cylinder 1 L;
- Laboratory grade thermometer (20 °C to 200 °C) with flask adapter;
- Top stirrer with heating plate;
- Laboratory scale (0.1 g-1 kg is suitable);
Note: the equipment list is the same for all methods.
m-Chloropropiophenone (3'-Chloropropiophenone) Synthesis
Reagents:- Ethyl magnesium bromide (2 L; 3M);
- m-chlorobenzonitrile (688 g; 5 mole);
- Ether (2.5 L);
- Hydrochloric acid (15%; 1305 ml; 5 mole);
- Methanol;
Procedures
1. To ethyl magnesium bromide (2 L; 3M) was added over 45 minutes with stir ring and cooling m-chlorobenzonitrile (688 g; 5 mole) in ether (2.5 L) in 10 L three-necked round bottom flask.
2. The resultant solution was heated under gentle reflux for 5 h.
3. The reaction-mixture was hydrolyzed with cold dilute hydrochloric acid (15%; 1305 ml; 5 mole), the ether was distilled off, and the aqueous solution was heated at 90°C for one hour.
4. The flask was then cooled to a room temperature and seded for a while. The solid ketone that separated was washed with cold water and recrystallized from methanol.
5. The recrystallized ketone m.p. is 39-40°C, weighed 750 g.
2. The resultant solution was heated under gentle reflux for 5 h.
3. The reaction-mixture was hydrolyzed with cold dilute hydrochloric acid (15%; 1305 ml; 5 mole), the ether was distilled off, and the aqueous solution was heated at 90°C for one hour.
4. The flask was then cooled to a room temperature and seded for a while. The solid ketone that separated was washed with cold water and recrystallized from methanol.
5. The recrystallized ketone m.p. is 39-40°C, weighed 750 g.
m-Fluoropropiophenone (3'-Fluoropropiophenone) Synthesis
Reagents:- Ethyl magnesium bromide (2 L; 3M);
- m-fluorobenzonitrile (605.6 g; 5 mole);
- Ether (2.5 L);
- Hydrochloric acid (15%; 1305 ml; 5 mole);
- Methanol;
Procedures
1. To ethyl magnesium bromide (2 L; 3M) was added over 45 minutes with stir ring and cooling m-fluorobenzonitrile (605.6 g; 5 mole) in ether (2.5 L) in 10 L three-necked round bottom flask.
2. The resultant solution was heated under gentle reflux for 5 h.
3. The reaction-mixture was hydrolyzed with cold dilute hydrochloric acid (15%; 1305 ml; 5 mole), the ether was distilled off, and the aqueous solution was heated at 90°C for one hour.
4. The flask was then cooled to a room temperature and seded for a while. The solid ketone that separated was washed with cold water and recrystallized from methanol.
5. 3'-Fluoropropiophenone boils at 89° C at 8 mm (vacuum distillation) pressure and melts at 29-30 °C.
2. The resultant solution was heated under gentle reflux for 5 h.
3. The reaction-mixture was hydrolyzed with cold dilute hydrochloric acid (15%; 1305 ml; 5 mole), the ether was distilled off, and the aqueous solution was heated at 90°C for one hour.
4. The flask was then cooled to a room temperature and seded for a while. The solid ketone that separated was washed with cold water and recrystallized from methanol.
5. 3'-Fluoropropiophenone boils at 89° C at 8 mm (vacuum distillation) pressure and melts at 29-30 °C.
Source
- Mehta, N. "Meta chloro substituted-alpha-butylamino-propiophenones." U.S. Patent No. 3,819,706. 25 Jun. 1974. https://patents.google.com/patent/US3819706A/en
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