HRID1348955
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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
To a solution of 2-amino-3-oxo-butyric acid methyl ester (100 mmol) (Lida, H. et al. Synthetic Communication, 1973, 3, 225–230) in 150 mL of ethanol was added KOCN (16.2 g, 200 mmol). The mixture was heated at 80° C. for 2 h. The solution was acidified with 2 N HCl and concentrated to half of the volume in vacuo. The product precipitated out upon cooling. Filtration, followed by washing with water, provided 5-methyl-2-oxo-2,3-dihydro-1H-imidazole-4-carboxylic acid methyl ester 4a (15 g, >95%). MS (ESI+) (M+1)=157.
WORKUP
后处理
- concentrationconcentrated to half of the volume in vacuo
- customThe product precipitated out
- temperatureupon cooling
- filtrationFiltration
- washby washing with water