HRID1291931

反应详情

EQUATION

反应方程式

HRID 1291931 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-(2-chloro-5-pyridyl)ethylamine (4.7 g), 1,1-bis-methylthio-2-nitroethylene (5.0 g) and ethanol (50 ml) was refluxed under heating until the generation of mercaptan ceased. Then, the ethanol was distilled off from the mixture under reduced pressure and the resulting residue was purified on a chromatographic column (the eluent mixture=ethanol+chloroform) to obtain the desired 1-{1-(2-chloro-5-pyridyl)ethylamino}-1-methylthio-2-nitroethylene (3.3 g) having a melting point in the range of from 136° to 140° C.

WORKUP

后处理

  1. temperaturewas refluxed
  2. distillationThen, the ethanol was distilled off from the mixture under reduced pressure
  3. customthe resulting residue was purified on a chromatographic column (the eluent mixture=ethanol+chloroform)