HRID1161693
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
To a solution of compound 4-(2-amino-6-phenyl-pyrimidin-4-ylamino)-2-chloro-phenol (0.5 g, 1.6 mmol) in dry dimethylformamide (10 mL) was added 4-(N,N-dimethylamino)pyridine (0.39 g, 3.2 mmol) at 0° C. with stirring under nitrogen atmosphere. To this was added freshly prepared succinyl chloride (0.62 g, 4 mmol). The mixture was then stirred at 80° C. for 20 hours. After completion of the reaction the mixture was diluted with water (75 mL), the solid separated was filtered off, washed with cold water (200 mL) and dried. The solid was purified further by column chromatography using petroleum ether-ethyl acetate to give the desired product as a light brown solid.
WORKUP
后处理
- stirringThe mixture was then stirred at 80° C. for 20 hours
- customAfter completion of the reaction the mixture
- customthe solid separated
- filtrationwas filtered off
- washwashed with cold water (200 mL)
- customdried
- customThe solid was purified further by column chromatography