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Bromination of 4-methylpropiophenone with bromine in methylene chloride or glacial acetic acid

William Dampier

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Reagents:
4-methylpropiophenone - 1000g
Methylene chloride - 3000ml
Bromine - 1080g
Sodium bicarbonate
Water

Safety precautions when working with bromine:
Bromine evaporates orange-red couples having a sharp smell. After contact with skin, bromine is rapidly absorbed and cause a long time does not heal burns and sores. A pair of bromine in contact with mucous membranes, causing a burning sensation in the nose and throat. Measuring the required amount of bromine and the execution of syntheses with its participation is necessarily carried out in an exhaust cabinet, with the use of rubber gloves and protective glasses or masks. Bromine, intended for synthesis, should be poured into a flat-bottomed flask through a conical funnel, fixed above the flask in the tripod ring. The spout of the funnel must be inside the flask and be significantly already its throat (so as not to make the air outlet when filling the flask bromine). From the crane and clutches of the drip funnel, it is necessary to thoroughly remove the lubricant from grinding surfaces and lubricate them with phosphoric acid.

Synthesis in DCM:
1. In the flask, add 1000 g 4-methylpropyophenone.
2. Poured 3000 ml of methylene chloride and stirred for 5 minutes.
3. Stop stirring.
4. 1080 g (348 ml) liquid bromine was added to the drip funnel.
5. In the flask from the funnel we rush 30-50 ml bromine.
6. We wait until all the bromine will be at the bottom.
7. The bromine must be dissolved on the bottom, and the mixture was discolored.
8. If this did not happen within 15-30 minutes, heating a mixture (just over 30 *С).
9. How bromine was dissolved, mix the mixture slightly and stop the stirring again.
10. Add a second, smaller portion of bromine to the mixture. After discoloration, stirring again.
11. We add the third, even less portion of bromine to the mixture. After discoloration, stirring again.
12. If the bromine dissolves immediately, we turn on the mixing to constant and continue dropwise, not by portions.
13. After adding, all the bromine was stirred for another half an hour.
14. Pour a saturated soda solution of water and mix for 5 minutes. Separate the water (aqueous layer from above).
15. Pour clean water, mix the mixture for 5 minutes, separate water (from above).
16. If we need a dry bromoketone, distill all chloride methylene from the flask with a straight condenser.
17. If you plan to methaminetion in methylene chloride, the mixture was left for further reaction, taking the yield bromoketone - 1500 g.

Synthesis in Acetic acid:
1. We repeat steps 1-13 of the previous synthesis, only replace the methylene chloride to acetic acid.
2. After gradually poured at least 3 liters of pure cold water and stirring.
3. In the process of pouring water and stirring the mixture, bromoketone crystallizes.
4. Filter the liquid through the flask with a fine mesh (sieve) or squeeze vacuum filtration through a Buchner funnel.
5. Washed a second time with soda water, filter and wash with clean water followed.
6. Filter bromoketone on vacuum, and drying to constant mass.
 
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KHaafii

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Reagents:
4-methylpropiophenone - 1000g
Methylene chloride - 3000ml
Bromine - 1080g
Sodium bicarbonate
Water

Safety precautions when working with bromine:
Bromine evaporates orange-red couples having a sharp smell. After contact with skin, bromine is rapidly absorbed and cause a long time does not heal burns and sores. A pair of bromine in contact with mucous membranes, causing a burning sensation in the nose and throat. Measuring the required amount of bromine and the execution of syntheses with its participation is necessarily carried out in an exhaust cabinet, with the use of rubber gloves and protective glasses or masks. Bromine, intended for synthesis, should be poured into a flat-bottomed flask through a conical funnel, fixed above the flask in the tripod ring. The spout of the funnel must be inside the flask and be significantly already its throat (so as not to make the air outlet when filling the flask bromine). From the crane and clutches of the drip funnel, it is necessary to thoroughly remove the lubricant from grinding surfaces and lubricate them with phosphoric acid.

Synthesis in DCM:
1. In the flask, add 1000 g 4-methylpropyophenone.
2. Poured 3000 ml of methylene chloride and stirred for 5 minutes.
3. Stop stirring.
4. 1080 g (348 ml) liquid bromine was added to the drip funnel.
5. In the flask from the funnel we rush 30-50 ml bromine.
6. We wait until all the bromine will be at the bottom.
7. The bromine must be dissolved on the bottom, and the mixture was discolored.
8. If this did not happen within 15-30 minutes, heating a mixture (just over 30 *С).
9. How bromine was dissolved, mix the mixture slightly and stop the stirring again.
10. Add a second, smaller portion of bromine to the mixture. After discoloration, stirring again.
11. We add the third, even less portion of bromine to the mixture. After discoloration, stirring again.
12. If the bromine dissolves immediately, we turn on the mixing to constant and continue dropwise, not by portions.
13. After adding, all the bromine was stirred for another half an hour.
14. Pour a saturated soda solution of water and mix for 5 minutes. Separate the water (aqueous layer from above).
15. Pour clean water, mix the mixture for 5 minutes, separate water (from above).
16. If we need a dry bromoketone, distill all chloride methylene from the flask with a straight condenser.
17. If you plan to methaminetion in methylene chloride, the mixture was left for further reaction, taking the yield bromoketone - 1500 g.

Synthesis in Acetic acid:
1. We repeat steps 1-13 of the previous synthesis, only replace the methylene chloride to acetic acid.
2. After gradually poured at least 3 liters of pure cold water and stirring.
3. In the process of pouring water and stirring the mixture, bromoketone crystallizes.
4. Filter the liquid through the flask with a fine mesh (sieve) or squeeze vacuum filtration through a Buchner funnel.
5. Washed a second time with soda water, filter and wash with clean water followed.
6. Filter bromoketone on vacuum, and drying to constant mass.
First of all thanks for the information.

I was curious about the following.

Solution of water with sodium carbonate. What percentage of sodium carbonate should this solution consist of or is recommended. How much liters should be added?

The following Once this synthesis is complete. Can I store this solution of bromine with 4 Methypropiophenone ( 2-Bromo-4'-methylpropiophenone ) in liquid form and use it immediately when synergizing mephedrone?

Can I safely store this 2-component solution in a HDPE material jerrycan or need i some stronger matrial?
 

William Dampier

Well-known member
Expert
Joined
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Messages
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Points
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Solution of water with sodium carbonate. What percentage of sodium carbonate should this solution consist of or is recommended. How much liters should be added?
When the pH of washing water is 6 or alkali
The following Once this synthesis is complete. Can I store this solution of bromine with 4 Methypropiophenone ( 2-Bromo-4'-methylpropiophenone ) in liquid form and use it immediately when synergizing mephedrone?
Yes
Can I safely store this 2-component solution in a HDPE material jerrycan or need i some stronger matrial?
For DCM solutions u must use glass bottles
 
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