反应详情

To a solution of 1-benzothiophen-6-amine 1,1-dioxide (1.00 g, 5.52 mmol) and pyridine (0.525 ml, 6.62 mmol) in tetrahydrofuran (18 ml) was added, under ice-cooling, 2,2,2-trichloroethyl chloroformate (0.916 ml, 6.62 mmol), and the mixture was stirred at room temperature for 1 hour and half. Water was poured to the reaction mixture, and the resulting solution was extracted with ethyl acetate. The extract was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. Hexane was poured to the residue, and 1.71 g (87.1%) of the desired product as a solid was separated by filtration.

1. temperaturecooling
2. extractionthe resulting solution was extracted with ethyl acetate
3. washThe extract was washed with water
4. dry with materialdried over anhydrous magnesium sulfate
5. distillationthe solvent was distilled off under reduced pressure
6. additionHexane was poured to the residue, and 1.71 g (87.1%) of the desired product as a solid
7. customwas separated by filtration