反应详情

温度

75 °C

A mixture of 800 mg of methyl 7-(trifluoromethyl)benzo[b]thiophene-2-carboxylate, 154 mg of lithium hydroxide monohydrate, 4 ml of water and 12 ml of methanol was stirred at 75° C. for 2 hours. The reaction mixture was cooled to room temperature, and then concentrated under reduced pressure. To the residue was added water, and then washed with tert-butyl methyl ether 3 times. To the aqueous layer was added concentrated hydrochloric acid, and then extracted with tert-butyl methyl ether 3 times. The combined organic layer was washed with saturated aqueous sodium chloride solution, dried over magnesium sulfate, and then concentrated under reduced pressure to obtain 632 mg of 7-(trifluoromethyl)benzo[b]thiophene-2-carboxylic acid (the present compound 4).

1. temperatureThe reaction mixture was cooled to room temperature
2. concentrationconcentrated under reduced pressure
3. additionTo the residue was added water
4. washwashed with tert-butyl methyl ether 3 times
5. additionTo the aqueous layer was added concentrated hydrochloric acid
6. extractionextracted with tert-butyl methyl ether 3 times
7. washThe combined organic layer was washed with saturated aqueous sodium chloride solution
8. dry with materialdried over magnesium sulfate
9. concentrationconcentrated under reduced pressure