HRID1596559

反应详情

EQUATION

反应方程式

HRID 1596559 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

8.1 g of phenylsulphonyl chloride were added at 0° C. to a solution of 10 g of (1b) in 100 ml of pyridine. After a reaction time of 15 min, 6.3 ml of triethylamine were added and the mixture was stirred at room temperature. After 5 h, it was concentrated, treated with 1 N HCl, extracted with dichloromethane, dried over MgSO4 and concentrated. Chromatographic purification (dichloromethane/methanol=5:1) yielded 11.4 g of a white solid.

WORKUP

后处理

  1. concentrationit was concentrated
  2. additiontreated with 1 N HCl
  3. extractionextracted with dichloromethane
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated
  6. customChromatographic purification (dichloromethane/methanol=5:1)