HRID724964

反应详情

EQUATION

反应方程式

HRID 724964 的结构方程式

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

The 2-chloro-5,11-dihydro-11-ethyl-5-methyl-8-vinyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (2.34 g, 7.43 mmol) was dissolved in 1:1 dichloromethane/methanol (40 mL) and cooled to -78° C. This solution was then saturated with ozone and a stream ozone was bubbled through for 10 minutes while stirring. The mixture was warmed to ambient temperature and quenched with excess dimethylsulfide. The mixture was then concentrated and the resulting residue was purified by flash chromatography (gradient of hexanes to 1:1 hexanes/ethyl acetate) to give the title compound (1.9 g, 81%), m.p. 199°-201° C.

WORKUP

后处理

  1. customsaturated with ozone and a stream ozone was bubbled through for 10 minutes
  2. temperatureThe mixture was warmed to ambient temperature
  3. customquenched with excess dimethylsulfide
  4. concentrationThe mixture was then concentrated
  5. customthe resulting residue was purified by flash chromatography (gradient of hexanes to 1:1 hexanes/ethyl acetate)