HRID2101682

反应详情

EQUATION

反应方程式

HRID 2101682 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Oxone (0.22 g) was added portionwise to a stirred solution of Example 575 (0.035 g) in N,N-dimethylformamide (4 ml). The mixture was stirred at room temperature under nitrogen for 24 h, a further portion of oxone (0.17 g) was added, and the mixture stirred for a further 5 h. The reaction was quenched with a solution of sodium sulphite (1.2 g) in water (15 ml), diluted with water (10 ml) and extracted with ethyl acetate (3×30 ml). The combined organic extracts were dried over magnesium sulphate and concentrated in vacuo to give the title compound as a buff solid (0.035 g).

WORKUP

后处理

  1. stirringthe mixture stirred for a further 5 h
  2. customThe reaction was quenched with a solution of sodium sulphite (1.2 g) in water (15 ml)
  3. additiondiluted with water (10 ml)
  4. extractionextracted with ethyl acetate (3×30 ml)
  5. dry with materialThe combined organic extracts were dried over magnesium sulphate
  6. concentrationconcentrated in vacuo