反应详情

温度

-20 °C

350 mg of 6,8,9,10,10a,11-hexahydro-3-methyl-1-phenyl-1H-oxazolo(5,4,3-jk)pyrrolo(2,1-C)(1,4)benzodiazepin-6,11-dione was treated in the same manner as in Example 4. The concentrate of the chloroform layer obtained was dissolved in 2 ml of hot ethanol, cooled to -20° C., and allowed to stand at this temperature for 3 days. Thus, 86 mg of 2,3,5,10,11,11a-hexahydro-11-ethoxy-9-hydroxy-8-methyl-1H-pyrrolo(2,1-C)(1,4)benzodiazepin-5-one was obtained in a colorless crystalline form. Recrystallization of the resulting product from ethanol gave a colorless needle-like crystal having a melting point of 155° to 157° C.

1. concentrationThe concentrate of the chloroform layer
2. customobtained