HRID15156

反应详情

EQUATION

反应方程式

HRID 15156 的结构方程式

PROCEDURE

实验过程

A solution of 3,8-difluoro-4-methylidene-4,5-dihydro-7H-pyrrolo[3,2,1-de]-1,5-naphthyridin-7-one (219 mg, 1 mmol) in tert-butanol/water (10 ml/10 ml) was treated with AD mix alpha/beta (0.75 g/0.75 g). After 6 hours the reaction mixture was treated with saturated sodium sulphite solution (10 ml). After 10 minutes the mixture was extracted with 20% methanol in dichloromethane (3×200 ml). The aqueous phase was concentrated (to ca 20 ml) and further extracted with 20% methanol in dichloromethane (3×200 ml). The organic extracts were dried and evaporated affording a white solid (206 mg, 82%).

WORKUP

后处理

  1. additionmix alpha/beta (0.75 g/0.75 g)
  2. extractionAfter 10 minutes the mixture was extracted with 20% methanol in dichloromethane (3×200 ml)
  3. concentrationThe aqueous phase was concentrated (to ca 20 ml)
  4. extractionfurther extracted with 20% methanol in dichloromethane (3×200 ml)
  5. customThe organic extracts were dried
  6. customevaporated