HRID1755681
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureunder refluxing for 5 hours
- concentrationThe reaction mixture was concentrated
- customthe residue was purified by column chromatography (
- washeluting solvent