HRID980123

反应详情

EQUATION

反应方程式

HRID 980123 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

23 g of compound (6) prepared above was suspended in 300 ml of chloroform and, while keeping the solution at 5°-10° C., 27.4 g of sulfuryl chloride was slowly dropwise added thereto. After reacting for 1.5 hours, water was added to the reaction solution to conduct separation and extraction. The organic phase was dried with anhydrous sodium sulfate, and chloroform was distilled off under reduced pressure. Rapid purification of the residue through silica gel column chromatography gave compound (7) as crystals. Yield: 8.8 g (33%).

WORKUP

后处理

  1. customat 5°-10° C.
  2. customseparation and extraction
  3. dry with materialThe organic phase was dried with anhydrous sodium sulfate, and chloroform
  4. distillationwas distilled off under reduced pressure
  5. customRapid purification of the residue through silica gel column chromatography