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