HRID514701

反应详情

EQUATION

反应方程式

HRID 514701 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-15 °C

PROCEDURE

实验过程

A solution of sodium methoxide (15.5 mL, 25 wt % in methanol) was diluted with methanol (85 mL) and treated with 2-propanethiol (6.3 mL) at room temperature for 60 minutes, cooled to −15° C., treated with 3-nitrobenzylchloride (10 g) in 3 portions, kept for 2 hours at −15° C., then the temperature was increased to room temperature. The reaction mixture was concentrated in vacuo, treated with diethyl ether (300 mL), washed with water (2×100 mL) and brine (100 mL), dried with sodium sulfate and evaporated to dryness. The title compound (12.3 g) was thus obtained and used without further purification.

WORKUP

后处理

  1. temperaturethe temperature was increased to room temperature
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. additiontreated with diethyl ether (300 mL)
  4. washwashed with water (2×100 mL) and brine (100 mL)
  5. dry with materialdried with sodium sulfate
  6. customevaporated to dryness