HRID724964
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- customsaturated with ozone and a stream ozone was bubbled through for 10 minutes
- temperatureThe mixture was warmed to ambient temperature
- customquenched with excess dimethylsulfide
- concentrationThe mixture was then concentrated
- customthe resulting residue was purified by flash chromatography (gradient of hexanes to 1:1 hexanes/ethyl acetate)