HRID1244934

反应详情

EQUATION

反应方程式

HRID 1244934 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The operation is carried out as in Stage 1 of Example 10 starting from 280 mg of the product obtained in Stage 1 of Example 7, 4 ml of methylene chloride, 0.2 ml of triethylamine and 248 mg of 4-methoxy-benzenesulphonic acid chloride in place of the 4-methyl-benzenesulphonic acid chloride then agitation is carried out at ambient temperature for approximately one night. Then 2 ml of water is added, followed by extracting with 3×5 ml of methylene chloride, washing with 5 ml of saturated sodium chloride, drying, evaporating, impasting in 5 ml of ether then in 5 ml of pentane, separating, and drying. After chromatography on silica eluting with methylene chloride/CH3CN in a proportion of 70/30, 250 mg of expected product is thus obtained in the form of a beige solid.

WORKUP

后处理

  1. waitthen agitation is carried out at ambient temperature for approximately one night
  2. extractionby extracting with 3×5 ml of methylene chloride
  3. washwashing with 5 ml of saturated sodium chloride
  4. customdrying
  5. customevaporating
  6. customin 5 ml of pentane, separating
  7. customdrying