HRID1755681

反应详情

EQUATION

反应方程式

HRID 1755681 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

A mixture of 1-[N-(6-chloro-3-pyridylmethyl)-N-ethylamino]-1-methylamino-2-nitroethylene (2.71 g), p-chlorothiophenol (1.45 g), 37% aqueous solution of formaldehyde (0.97 g) and ethanol (30 ml) was stirred at 20° C. for 2 hours and under refluxing for 5 hours. The reaction mixture was concentrated and the residue was purified by column chromatography (eluting solvent:dichloromethane-methanol (6:1) to give 3-(4-chlorophenylthio)-1-[N-(6-chloro-3-pyridylmethyl)-N-ethylamino]-1-methylamino-2-nitro-1-propene (Compound No. 31) (3.30 g) as a yellow amorphous.

WORKUP

后处理

  1. temperatureunder refluxing for 5 hours
  2. concentrationThe reaction mixture was concentrated
  3. customthe residue was purified by column chromatography (
  4. washeluting solvent