反应详情

A mixture of (3RS,5RS,αRS)-7-chloro-5-(2-chlorophenyl)-1-isopropyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-glycolic acid (0.15 g) obtained in Example 7, p-toluenesulfonic acid monohydrate (7 mg) and ethanol (20 ml) was heated for 24 hours under reflux. Ethanol was distilled off under reduced pressure. The residue was dissolved in a mixture of water (50 ml) and ethyl acetate (50 ml). The organic layer was washed with an aqueous solution of sodium hydrogencarbonate, which was dried over anhydrous magnesium sulfate, then the solvent was was distilled off under reduced pressure to leave (3RS,5RS,αRS)-7-chloro-5-(2-chlorophenyl)-1-isopropyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-glycolic acid ethyl ester (0.14 g) as prisms, m.p. 119°-120° C.

1. temperaturewas heated for 24 hours
2. temperatureunder reflux
3. distillationEthanol was distilled off under reduced pressure
4. dissolutionThe residue was dissolved in a mixture of water (50 ml) and ethyl acetate (50 ml)
5. washThe organic layer was washed with an aqueous solution of sodium hydrogencarbonate, which
6. dry with materialwas dried over anhydrous magnesium sulfate
7. distillationthe solvent was was distilled off under reduced pressure