HRID561901

反应详情

EQUATION

反应方程式

HRID 561901 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of toluene-4-sulfonic acid (S)-2-(3-chlorophenyl)-2-hydroxyethyl ester (16.34 g, 0.050 mol), sodium azide (6.50 g, 0.10 mol) and DMSO (50 mL) was stirred for 2 h at 80° C. Water (100 mL) was added, extracted with hexane-ether (1:1) mixture (2×150 mL). Combined extract was dried over Na2SO4, evaporated. The residue was separated on SiO2 (100 g), hexane-EtOAc, 0 to 20%. Colorless oil, 7.0 g, (0.035 mol, 71%).

WORKUP

后处理

  1. extractionextracted with hexane-ether (1:1) mixture (2×150 mL)
  2. extractionCombined extract
  3. dry with materialwas dried over Na2SO4
  4. customevaporated
  5. customThe residue was separated on SiO2 (100 g), hexane-EtOAc, 0 to 20%