HRID354879
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
- 155 °C
PROCEDURE
实验过程
A mixture of 4-amino-6-methanesulfonamidoquinazoline (6.89 g), diethyl ethoxymethylenepropanediate (15.5 g) and N,N-dimethylformamide (55 ml) was stirred at 155° C. for 2.5 hours. The reaction mixture was cooled to ambient temperature. To the mixture was added water to give precipitates, which were separated by filtration and washed with water. To the crystals was added a mixture of methanol and chloroform (1:4) (400 ml). After stirring under heating, insoluble materials (6.95 g) were filtered off and recrystallized from N,N-dimethylformamide to give crystalline ethyl 4-oxo-10-methanesulfonamido-4H-pyrimido [1,2-c]quinazoline-3-carboxylate (5.76 g).
WORKUP
后处理
- temperatureThe reaction mixture was cooled to ambient temperature
- customto give
- customprecipitates
- customwhich were separated by filtration
- washwashed with water
- additionTo the crystals was added
- additiona mixture of methanol and chloroform (1:4) (400 ml)
- stirringAfter stirring
- temperatureunder heating
- filtrationinsoluble materials (6.95 g) were filtered off
- customrecrystallized from N,N-dimethylformamide