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HRID1493313

反应详情

EQUATION

反应方程式

HRID 1493313 的结构方程式

REACTANTS

反应物

2
结构：N#CCCl
HCID7856

Chloroacetonitrile

C2H2ClN

结构：CCOC(=O)C1=C(CS)NC(C)=C(C#N)C1c1cccc([N+](=O)[O-])c1
HCID19831124

未命名化合物

PRODUCTS

生成物

1
结构：CCOC(=O)C1=C(CSCC#N)NC(C)=C(C#N)C1c1cccc([N+](=O)[O-])c1
HCID19831123

未命名化合物

收率 54.1%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CCO
溶剂HCID702

Ethanol

C2H6O

PROCEDURE

实验过程

A solution of 2-mercaptomethyl-3-carboethoxy-5-cyano-4-(m-nitrophenyl)-6-methyl-1,4-dihydropyridine (3 g), 2-chloroacetonitrile (1 g) and 1,4-diazabicyclo-2,2,2-octa ne (0.8 g) in EtOH (30 ml) is heated at reflux temperature for six hours. Then the reaction is cooled to room temperature and after usual work-up and purification by columnchromatography (SiO2 90 g; eluent Et2O/AcOEt 90/10) gives 1.8 g of 2-(cyanomethylthio)methyl-3-carboethoxy-5-cyano-4-(m-nitrophenyl)-6-methyl-1,4-dihydropyridine.

WORKUP

后处理

  1. temperatureat reflux temperature for six hours
  2. customafter usual work-up and purification by columnchromatography (SiO2 90 g; eluent Et2O/AcOEt 90/10)