HRID230857

反应详情

EQUATION

反应方程式

HRID 230857 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Oxone (0.5 g) was added portionwise to a stirred solution of Intermediate 64 (0.12 g) in N,N-dimethylformamide (5 ml). The solution was stirred at room temperature under nitrogen for 21 h. More oxone (0.5 g) was added and the mixture was stirred for a further 3 h, quenched with a solution of sodium sulphite (1.5 g) in water (15 ml), diluted with water (50 ml) and extracted with ethyl acetate (3×50 ml). The combined organic extracts were dried over magnesium sulphate and concentrated in vacuo to give the title compound as a yellow solid (0.15 g).

WORKUP

后处理

  1. stirringthe mixture was stirred for a further 3 h
  2. customquenched with a solution of sodium sulphite (1.5 g) in water (15 ml)
  3. additiondiluted with water (50 ml)
  4. extractionextracted with ethyl acetate (3×50 ml)
  5. dry with materialThe combined organic extracts were dried over magnesium sulphate
  6. concentrationconcentrated in vacuo