反应详情

A mixture of tert-butyl 9-(3,3-difluoropyrrolidin-1-yl)-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate (110 mg, 0.310 mmol), ethyl acetate (2 ml) and 4N hydrogen chloride-ethyl acetate solution (2 ml) was stirred at room temperature for 1 hr, and the solvent was evaporated under reduced pressure. The residue was added to 1N aqueous sodium hydroxide solution (2 ml), and the mixture was extracted with ethyl acetate:tetrahydrofuran (1:1). The extract was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by NH silica gel column chromatography (hexane:ethyl acetate=1:1) to give the desired product (41.0 mg, 52.0%) as a solid.

1. customthe solvent was evaporated under reduced pressure
2. additionThe residue was added to 1N aqueous sodium hydroxide solution (2 ml)
3. extractionthe mixture was extracted with ethyl acetate:tetrahydrofuran (1:1)
4. dry with materialThe extract was dried over anhydrous magnesium sulfate
5. customthe solvent was evaporated under reduced pressure
6. customThe residue was purified by NH silica gel column chromatography (hexane:ethyl acetate=1:1)