HRID2072677

反应详情

EQUATION

反应方程式

HRID 2072677 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of sodium (1.4 g) in ethanol (120 ml) was added malonamide (3.8 g) and the mixture was heated at 60° C. for an hour under stirring. Then after added N-(2-thenoyl)glycine ethyl ester (8 g), the mixture was refluxed for 6 hours. The mixture was concentrated to give the residue which was diluted with water. The aqueous mixture was neutralized by adding acetic acid to deposit a crystalline product which was collected by filtration and recrystallized from dimethylformamide (DMF) to give the objective product (2.8 g) as colorless crystals, mp 270°-275° C. (decompd.).

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 6 hours
  2. concentrationThe mixture was concentrated
  3. customto give the residue which
  4. filtrationwas collected by filtration
  5. customrecrystallized from dimethylformamide (DMF)