HRID1271032
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
A mixture of 0.7 g of 4-chloro-5-(4-chlorophenylethynyl)-2-diisopropylaminomethyleneamino-pyrimidine, 20 mL ethanol and 0.6 mL ethanolamine was refluxed for 18 hours. The green solution was evaporated in vacuo and triturated with water. The insoluble yellow residue was recrystallized by dissolving in 35 mL hot methanol, concentrating to 10 mL and chilling. The pale yellow powdery precipitate was filtered and dried to yield 0.34 g of 2-amino-5-(4-chlorophenylethynyl)-4-(2-hyroxyethylamino)pyrimidine, m.p. 197–200° C.
WORKUP
后处理
- temperaturewas refluxed for 18 hours
- customThe green solution was evaporated in vacuo
- customtriturated with water
- customThe insoluble yellow residue was recrystallized
- dissolutionby dissolving in 35 mL hot methanol
- concentrationconcentrating to 10 mL
- temperaturechilling
- filtrationThe pale yellow powdery precipitate was filtered
- customdried