HRID243541
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
1000 ml of dimethylformamide, 51.52 g of 3,5-dimethyl-4-hydroxybenzonitrile, 106.9 g of diazabicyclo undecene were added to a reaction vessel and stirred at RT. The reaction mixture was maintained at same temperature for 1 hr and 100 g of N-[5-bromo-6-chloro-2-(4-cyanophenylamino)-pyrimidin-4-yl]benzamide added with continued stirring for 30 mins. The reaction mixture was heated to 100-110° C. and further maintained at same temperature for 24 hr. After completion of the reaction, the reaction mixture was cooled to RT and 2000 ml of water added and stirred at RT for 1 hr. The reaction mixture was filtered. The obtained solid was dried under vacuum (0.5 kg/cm2) at 55-60° C. overnight.
WORKUP
后处理
- temperatureThe reaction mixture was maintained at same temperature for 1 hr
- stirringwith continued stirring for 30 mins
- temperatureThe reaction mixture was heated to 100-110° C.
- temperaturefurther maintained at same temperature for 24 hr
- customAfter completion of the reaction
- temperaturethe reaction mixture was cooled to RT
- stirringstirred at RT for 1 hr
- filtrationThe reaction mixture was filtered
- customThe obtained solid was dried under vacuum (0.5 kg/cm2) at 55-60° C. overnight