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2-Bromo-4'-methylpropiophenone synthesis from 4'-methylpropiophenone. Bromination in DCM or GAA.

William D.

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Reagents:
  • 4-methylpropiophenone (cas 5337-93-9) - 1000 g;
  • Dichloromethane (DCM) or glacial acetic acid (GAA) - 3000 ml;
  • Bromine (Br2) - 1080g, 348 ml;
  • Sodium bicarbonae (NaHCO3) solution;
  • Distilled water;
  • Magnesium sulphate (MgSO4);
Equipment and glassware:
Safety precautions when working with bromine:
Bromine has an orange-red fumes with a sharp smell. Bromine is rapidly absorbed by skin and caused hard long non-healing burns and ulcers. A bromine vapors are caused a burning sensation in nose and throat during contact with mucous membranes. All manipulations with bromine and syntheses have to be carried out in an exhaust fume hood with rubber gloves, protective googles and mask. Bromine should be poured into a flat-bottomed flask through a conical funnel, which is fixed above the flask on retort stand. A tip of the funnel must be inside of the flask. It is necessary to thoroughly remove a lubricant from grinding surfaces of crane and clutches of a drip funnel and clean them with phosphoric acid .

Synthesis in DCM:
1. 4-Methylpropyophenone 1000 g is placed into a 10 L flask.
2. Dichloromethane (DCM) 3000 ml is poured there and stirred for 5 min.
3. The stirring is stopped. Liquid bromine (Br2) 1080 g, 348 ml is added to a drip funnel.
4. Bromine (Br2) 30-50 ml is added dropwise into the flask from the drip funnel.
5. Bromine have to fall at the flask bottom.
6. Bromine must be dissolved on the bottom and the mixture have to be discolored.
7. The mixture is heated to 30 °C, if the solution isn't discolored.
8. The mixture slightly stirred and the stirring is stopped when bromine is dissolved.
9. A second smaller bromine portion is added to the mixture. It is stirred again after discoloration.
10. A third even less bromine portion is added to the mixture. It is stirred again after discoloration.
11. If bromine is dissolved immediately, bromine addition is continued dropwise, not by portions, with a constant stirring.
12. The reaction mixture is stirred 30 min after complete bromine addition.
13. A saturated sodium bicarbonae (NaHCO3) solution is added to the flask and stirred for 5 min. Then, layers are separated.
14. Distilled water is added to the organic layer, the mixture is stirred for 5 min. Layers are separated.
15. Organic layer is dried over
sodium sulphate (MgSO4) and filtered from solids. Organic solvent is distilled off with vacuum form the solution in case you need dry 2-bromo-4'-methylpropiophenone (cas 1451-82-7).
16. The mixture is left for further reaction with approximate 2-bromo-4'-methylpropiophenone (cas 1451-82-7) yield 1500 g in case you need to carry out methylamination in DCM.

Synthesis in Acetic acid:
1. Previous synthesis steps 1-12 are same, the DCM is replaced to acetic acid.
2. Cold distilled water 3 L is gradually poured to the mixture and stirred.
3. 2-Bromo-4'-methylpropiophenone (cas 1451-82-7) is crystallized during water addition and stirred.
4. The 2-bromo-4'-methylpropiophenone product is filtred on Buchner flask and funnel.
5. The product crystals are washed with sodium bicarbonae (NaHCO3) solution, filtered and washed again with distilled water to
neutral pH 6.5-7.
6. 2-Bromo-4'-methylpropiophenone (cas 1451-82-7) is filtered on Buchner flask and funnel, and air dried (or in vacuum desiccator) to a 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.
William DampierFirst 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 D.

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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?
KHaafiiWhen 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
 

Mellym

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Let me share a piece of my practical experience. With the acetic acid route it doesn't have to be glacial concentration. I've tried 70% "acetic essence", (that is available OTC in food stores in my area) and it worked!

BTW, the process is much less messy and easy workup compared to the DCM route.
 

little-flower

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Hello"" does anyone have a melting point for the 2bromo3methylpropiophenone?


I can't find it anywhere,

molecul symmetry of 2B4MP and 2B3MP are not the same,,
 

little-flower

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Has anyone ever recrystallized 2-bromo4'methylpropiophenone?
 
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little-flower

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StarWars

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Goku

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how much does it cost to produce on a large scale 2b4m 1kg costs $25 if you buy a lot of chemistry from china and produce it yourself
 

w2x3f5

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Bromination stuck when have much HBr inside
 
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