反应详情

In ethanol (8 ml) was dissolved (3RS,5SR,αSR)-7-chloro-5-(2-chlorophenyl)-1-isopropyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-glycolic acid ethyl ester (0.3 g) obtained in Example 1. To the solution was added 1N sodium hydroxide (2 ml), and the mixture was left standing for 20 minutes at room temperature. To the resultant mixture was added 1N hydrochloric acid (50 ml) to make the solution acid, followed by extraction with ethyl acetate (50 ml). The extract solution was washed with water, dried over anhydrous magnesium sulfate, then the solvent was distilled off under reduced pressure to give (3RS,5SR,αSR)-7-chloro-5-(2-chlorophenyl)-1-isopropyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-glycolic acid (0.26 g) as prisms, m.p. 245°-247° C. (decomp.).

1. waitthe mixture was left
2. extractionfollowed by extraction with ethyl acetate (50 ml)
3. washThe extract solution was washed with water
4. dry with materialdried over anhydrous magnesium sulfate
5. distillationthe solvent was distilled off under reduced pressure