反应详情

温度

0 °C

3-Amino-2-oxo-1-imidazolidinecarboxamide, monohydrochloride (12 g 0.006 mol) was suspended in 300 ml of dichloromethane. The suspension was cooled to 0° C. and 29.2 ml of triethylamine (0.198 mol) was added; the mixture was stirred for another 20 minutes. [3,4-Bis(acetyloxy)benzoyl]chloride (10.5 g) dissolved in 200 ml of dichloromethane was added dropwise with stirring at 0° C. and the mixture was stirred overnight at room temperature, filtered and treated with 50 ml of water. After stirring for 5 minutes, 3-[3,4-bis(acetyloxy)benzoyl]-2-oxo-1-imidazolidinecarboxamide crystallized out (7.2 g) contaminated with some triethylamine hydrochloride. The impurity was removed by treatment with water to yield 6.6 g of 3-[3,4-bis(acetyloxy)benzoyl]-2-oxo-1-imidazolidinecarboxamide, melting point 222°-224° C.

1. additionwas added dropwise
2. stirringwith stirring at 0° C.
3. stirringthe mixture was stirred overnight at room temperature
4. filtrationfiltered
5. additiontreated with 50 ml of water
6. stirringAfter stirring for 5 minutes
7. custom3-[3,4-bis(acetyloxy)benzoyl]-2-oxo-1-imidazolidinecarboxamide crystallized out (7.2 g)
8. customThe impurity was removed by treatment with water