HRID1156386

反应详情

EQUATION

反应方程式

HRID 1156386 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-Chloro-1-(m-nitrophenylsulfonyl)ethyl p-bromophenyl sulfide (27.1 g, 62.1 mmoles) was dissolved in 125 ml of tetrahydrofuran. The solution was diluted with 125 ml of diethyl ether and treated with 8.65 ml (6.3 g, 62.3 mmoles) of triethylamine. After one hour the mixture was filtered to remove 7.52 g (88%) of triethylamine hydrochloride, m.p. 255°-258°. Removal of solvent from the filtrate gave a yellow oil which crystallized upon scraping. Recrystallization from 25 ml of ethyl acetate and 10 ml of pentane gave 12 g (48%) of product m.p. 109°-111°.

WORKUP

后处理

  1. filtrationAfter one hour the mixture was filtered
  2. customto remove 7.52 g (88%) of triethylamine hydrochloride, m.p. 255°-258°
  3. customRemoval of solvent from the filtrate
  4. customgave a yellow oil which
  5. customcrystallized
  6. customRecrystallization from 25 ml of ethyl acetate and 10 ml of pentane