反应详情

温度

60 °C

A mixture of 5.0 g of 2-fluoro-5-(trifluoromethyl)benzaldehyde, 3.3 g of methyl thioglycolate, 4.0 g of potassium carbonate and 50 ml of DMF was stirred at 60° C. for 2 hours, and then the reaction mixture was cooled to room temperature. To the reaction mixture was added water, and extracted with tert-butyl methyl ether 3 times. The combined organic layer was washed with water, followed by saturated aqueous sodium chloride solution. The mixture was dried over magnesium sulfate, and then concentrated under reduced pressure. The residue was recrystallized from methanol to obtain 6.3 g of methyl 5-(trifluoromethyl)benzo[b]thiophene-2-carboxylate.

1. temperaturethe reaction mixture was cooled to room temperature
2. extractionextracted with tert-butyl methyl ether 3 times
3. washThe combined organic layer was washed with water
4. dry with materialThe mixture was dried over magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue was recrystallized from methanol