HRID1868479
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
A suspension of 2-amino-1H-imidazole-4-sulfonic acid (82 mg, 0.5 mmol) and 2-(2,4-dichlorobenzylidene)-3-oxobutanamide (125 mg, 0.5 mmol) in 3:1 EtOH/H2O (2 mL) was heated to 80° C. for 14 h. After removal of solvent, the residue was dissolved in 1N NaOH and extracted with EtOAc (5 mL×2). The aqueous solution was then acidified with conc. HCl to pH=1. The precipitation which had formed was collected and further washed with H2O. After drying in vacuo, 6-carbamoyl-5-(2,4-dichlorophenyl)-7-methyl-5,8-dihydroimidazo[1,2-a]pyrimidine-2-sulfonic acid was obtained a yellow solid (97 mg, 48%).
WORKUP
后处理
- customAfter removal of solvent
- dissolutionthe residue was dissolved in 1N NaOH
- extractionextracted with EtOAc (5 mL×2)
- customThe precipitation which
- customhad formed
- customwas collected
- washfurther washed with H2O
- customAfter drying in vacuo