反应详情

A mixture of (3RS,5SR,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 (6 mg) and ethanol (20 ml) was heated for 10 hours under reflux. Ethanol was distilled off under reduced pressure. To the residue were added water (50 ml) and ethyl acetate (50 ml). The organic layer was washed with an aqueous solution of sodium hydrogencarbonate, dried over anhydrous magnesium sulfate, followed by distilling off the solvent under reduced pressure to leave (3RS,5SR,αRS)-7-chloro-5-(2-chlorophenyl)-1-isopropyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-glycolic acid ethyl ester (95 mg) as prisms, m.p. 126°-128° C.

1. temperaturewas heated for 10 hours
2. temperatureunder reflux
3. distillationEthanol was distilled off under reduced pressure
4. additionTo the residue were added water (50 ml) and ethyl acetate (50 ml)
5. washThe organic layer was washed with an aqueous solution of sodium hydrogencarbonate
6. dry with materialdried over anhydrous magnesium sulfate
7. distillationby distilling off the solvent under reduced pressure