2-Bromo-5-methoxybenzotrifluoride synthesis
- Product Name:2-Bromo-5-methoxybenzotrifluoride
- CAS Number:400-72-6
- Molecular formula:C8H6BrF3O
- Molecular Weight:255.03
Yield:-
Reaction Conditions:
in N-methyl-acetamide;water
Steps:
2 2.
2. Preparation of 3-trifluoromethyl-4-bromo-1-methoxy-benzene (compound III) A solution prepared by dissolving 3-trifluoromethyl-4-bromo-1-phenol (4.4 g) in dehydrated dimethylformamide (20 ml) was added dropwise to a solution prepared by suspending 60% sodium hydride (0.86 g) in dehydrated dimethylformamide (10 ml) over a period of about 30 minutes at 25° C. or lower. Then, the mixture was stirred at room temperature for 30 minutes and then, methyl iodide (3.1 g) was slowly added thereto at 30° C. or lower and reaction was allowed to proceed at room temperature for 1 hour. Unreacted 60% sodium hydride was decomposed by conventional method and the reaction mixture was added to water (60 ml) and extracted with ethyl acetate and ethyl acetate layer was sufficiently washed with water and dehydrated by adding anhydrous sodium sulfate thereto. The solvent was removed by distillation under reduced pressure and the residue was purified by distillation to obtain 3-trifluoromethyl-4-bromo-1-methoxybenzene (compound III, 4.4 g).
References:
Showa Shell Sekiyu Kabushiki Kaisha US5183934, 1993, A
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400-72-6
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