HRID1290650

反应详情

EQUATION

反应方程式

HRID 1290650 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution containing 0.688 g of ethyl 2-aminothiazole-4carboxilate (prepared as reported in J.A.C.S. 68,266,1946) and 0.3 g of 2-bromoacrylic acid in 10 ml of dioxane, 0.412 g of N-N'dicyclohexylcarbodiimide were and the mixture was stirred at room temperature overnight. After filtration, the solvent was evaporated in vacuo, the solid residue was dissolved in 50 ml of ethyl acetate, treated with saturated solution of sodium bicarbonate and then with 10% hydrochloric acid. The organic phase was dried over anhydrous sodium sulphate and the solvent evaporated in vacuo. The solid residue was purified by recrystallization from ethanol-water to yield 0.52 g of ethyl 2-(α-bromoacrylamido)thiazole-4-carboxylate.

WORKUP

后处理

  1. filtrationAfter filtration
  2. customthe solvent was evaporated in vacuo
  3. dissolutionthe solid residue was dissolved in 50 ml of ethyl acetate
  4. additiontreated with saturated solution of sodium bicarbonate
  5. dry with materialThe organic phase was dried over anhydrous sodium sulphate
  6. customthe solvent evaporated in vacuo
  7. customThe solid residue was purified by recrystallization from ethanol-water