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
- 59 °C
PROCEDURE
实验过程
1350 ml of acetonitrile was taken into a RB flask at 27±3° C. To this was added 900 ml of IPA. To the reaction mixture 150 g of N-[5-bromo-6-(4-cyano-2,6-dimethylphenoxy)-2-(4-cyano-phenylamino)pyrimidin-4-yl]benzamide and 35.2 g of lithium hydroxide monohydrate were added and heated to 59±3° C. The reaction mixture was maintained at the same temperature for 10 hrs. After completion of the reaction, the reaction mixture was cooled to 47±3° C. and filtered. The solid was washed with acetonitrile and suck dried. The wet cake was taken into another flask to which was added 1500 ml of water, stirred for 30 mins and filtered to obtain the solid. The solid was washed with water and dried under vacuum at 73±3° C. to isolate Etravirine.
WORKUP
后处理
- customwas taken into a RB flask at 27±3° C
- temperatureThe reaction mixture was maintained at the same temperature for 10 hrs
- customAfter completion of the reaction
- temperaturethe reaction mixture was cooled to 47±3° C.
- filtrationfiltered
- washThe solid was washed with acetonitrile and suck
- customdried
- customThe wet cake was taken into another flask to which
- additionwas added 1500 ml of water
- filtrationfiltered
- customto obtain the solid
- washThe solid was washed with water
- customdried under vacuum at 73±3° C.