HRID727444

反应详情

EQUATION

反应方程式

HRID 727444 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 2.42 g (9.2 mmol) of triphenylphosphine in 5 ml of dichloromethane is added dropwise, at 0° C. under a nitrogen atmosphere, 0.70 ml (8.8 mmol) of sulphuryl chloride. The reaction medium is left stirring for 10 minutes at 0° C., followed by addition over 5 minutes of a solution containing 1.06 g (4.4 mmol) of 2-amino-3-cyclopentylbenzenesulphonic acid and 1.04 ml of tributylamine in 3 ml of dichloromethane. The mixture is brought to room temperature and is left at this temperature for 2 hours, then it is purified by chromatography on a column of silica gel, eluting with a dichloromethane/pentane mixture (1:1).

WORKUP

后处理

  1. waitThe reaction medium is left
  2. additionfollowed by addition over 5 minutes of a solution
  3. customis brought to room temperature
  4. waitis left at this temperature for 2 hours
  5. customit is purified by chromatography on a column of silica gel
  6. washeluting with a dichloromethane/pentane mixture (1:1)