HRID1492766
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
Ethyl 2-amino-3-oxobutanoate hydrochloride (10 g) was added to a stirring solution of ethyl butaneimidate (83.5 g) in ethanol (800 ml, freshly distilled from magnesium ethoxide) and triethylamine (85 ml) and the resultant yellow mixture stirred at room temperature for 48 h. The solvent was removed in vacuo and the residue diluted with water (500 ml) and extracted into ethyl acetate (3×200 ml). The combined organic extracts were washed with water (2×100 ml), dried and concentrated in vacuo. The resultant residue was purified by trituration with ether (5×50 ml) and the residual buff solid dried to afford the title compound (4.05 g)
WORKUP
后处理
- distillationfreshly distilled from magnesium ethoxide) and triethylamine (85 ml)
- customThe solvent was removed in vacuo
- additionthe residue diluted with water (500 ml)
- extractionextracted into ethyl acetate (3×200 ml)
- washThe combined organic extracts were washed with water (2×100 ml)
- customdried
- concentrationconcentrated in vacuo
- customThe resultant residue was purified by trituration with ether (5×50 ml)
- customthe residual buff solid dried