HRID726745

反应详情

EQUATION

反应方程式

HRID 726745 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of (0.5 g) of 2-nitrothiophen-5-carboxaldehyde and (0.7 g) of sulfonyl diacetonitrile in 6 mL ethanol was refluxed with a few drops of piperidine for 4 hours. Ethanol was removed in a rotavap and the mixture worked up with ethylacetate, diluted acid and brine. A portion of the crude was then purified by HPLC on a C-18 column to provide (0.05 g) of (E)-2-cyanomethylsulfonyl-3-(2-nitrothien-5-yl)acrylonitrile along with (0.03 g) of (E,E)-2-[[1-cyano-2-(2-nitrothien-5-yl)ethenyl]sulfonyl]-3-(2-nitrothien-5-yl)acrylonitrile.

WORKUP

后处理

  1. customEthanol was removed in a rotavap
  2. additiondiluted acid and brine
  3. customA portion of the crude was then purified by HPLC on a C-18 column