HRID745158

反应详情

EQUATION

反应方程式

HRID 745158 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 117.97 g (0.53 mole) of 2-[(3,4-dichlorophenyl)thio]ethanol (prepared by reacting 3,4-dichlorothiophenol and 2-chloroethanol) and 53.5 g (0.53 mole) of triethylamine in 500 ml of benzene was added dropwise a benzene solution of 60.9 g (0.53 mole) of methanesulfonyl chloride over a one hour period with cooling in an ice bath. The reaction mixture was stirred at room temperature overnight and filtered. Solvent was removed from the filtrate in a rotary evaporator to give an oil which crystallized. A portion was recrystallized from isopropyl ether to give white crystalline solid, m.p. 53°-55° C.

WORKUP

后处理

  1. temperaturewith cooling in an ice bath
  2. filtrationfiltered
  3. customSolvent was removed from the filtrate in a rotary evaporator
  4. customto give an oil which
  5. customcrystallized
  6. customA portion was recrystallized from isopropyl ether
  7. customto give white crystalline solid, m.p. 53°-55° C.