HRID1098755

反应详情

EQUATION

反应方程式

HRID 1098755 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of the product obtained from step 2 (1.38 g, 5.10 mmol) in methanol (25 ml) and tetrahydrofurane (25 ml) was added drop wise to a solution of oxone (5.64 g, 9.17 mmol) in water (25 ml) at 0° C. The suspension was stirred 2 days at RT. Water (25 ml) was added and the reaction mixture was extracted with DCM. The combined organic phases were washed with brine and dried over magnesium sulphate. Evaporation and purification of the crude product by silica gel chromatography using ethyl acetate/n-heptane gave the desired product (1.04 g, 67%).

WORKUP

后处理

  1. extractionthe reaction mixture was extracted with DCM
  2. washThe combined organic phases were washed with brine
  3. dry with materialdried over magnesium sulphate
  4. customEvaporation and purification of the crude product by silica gel chromatography