HRID1644553

反应详情

EQUATION

反应方程式

HRID 1644553 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1.192 mmol of thiophosgene in 5 ml of methylene chloride was added to an aqueous solution of 2.71 mmol of sodium bicarbonate. Then, over the course of 15 minutes, a mixture of 1.084 mmol of 2-(3-chlorophenyl)-2-(4-nitrophenyl)ethylamine was added dropwise to this mixture. After removal of the organic phase and extraction of the aqueous phase once again with dichloromethane, the combined organic phases were washed with water and the solvent was removed by distillation under reduced pressure in a Rotavapor. The reddish oily 2-(3-chlorophenyl)-2-(4-nitrophenyl)ethyl isothiocyanate was stored in a closed vessel with exclusion of moisture in a refrigerator until processed further.

WORKUP

后处理

  1. additionwas added dropwise to this mixture
  2. customAfter removal of the organic phase and extraction of the aqueous phase once again with dichloromethane
  3. washthe combined organic phases were washed with water
  4. customthe solvent was removed by distillation under reduced pressure in a Rotavapor
  5. customThe reddish oily 2-(3-chlorophenyl)-2-(4-nitrophenyl)ethyl isothiocyanate was stored in a closed vessel with exclusion of moisture in a refrigerator