HRID33492

反应详情

EQUATION

反应方程式

HRID 33492 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-30 °C

PROCEDURE

实验过程

1.58 g (6.14 mmol) (4-allyloxy-phenyl)-methanethiol and 1.64 g (6.14 mmol) toluene-4-sulfonic acid 2-[1,2,3]triazol-1-yl-ethyl ester were dissolved in 15 ml N,N-dimethylformamide (DMF) and cooled to −30° C. 294 mg (12.3 mmol) 95% Sodium hydride were added, the mixture allowed to warm to room temperature (r.t.) and stirred for 12 h. 10 ml Water were added and the residue dissolved in dichloromethane. The organic phase was dried over Na2SO4, solvents removed and the remaining material purified by chromatography on silica gel (ethyl acetate/n-heptane 1:1) to yield 1.33 g (79%) yellow oil.

WORKUP

后处理

  1. temperatureto warm to room temperature (r.t.)
  2. dry with materialThe organic phase was dried over Na2SO4, solvents
  3. customremoved
  4. customthe remaining material purified by chromatography on silica gel (ethyl acetate/n-heptane 1:1)