反应详情

1500 ml of dichloromethane and 150 g of N-[6-chloro-2-(4-cyanophenylamino)pyrimidin-4-yl]benzamide were added to a reaction vessel and to this was added 750 ml of acetic acid and 44.2 mL of liquid bromine solution at 27±3° C. and stirred for 11 hrs. After completion of the reaction, to the reaction mixture was added 375 ml of water under stirring and maintained for 45 mins. To the reaction mixture was further added metabisulphate solution (60 g in 375 ml of water) and stirred further for 30 mins. The solid was filtered and washed with 300 ml of water and suck dried. The wet cake and 1500 ml of water were charged into a clean RB and adjusted pH 9.0±0.5 with 50% potassium carbonate solution. The reaction mass was stirred and filtered; the solid was washed with 150 ml of water followed by 150 ml of dichloromethane. The obtained solid was dried under vacuum at 73±2° C. to yield the title compound.

1. customAfter completion of the reaction
2. stirringunder stirring
3. temperaturemaintained for 45 mins
4. stirringstirred further for 30 mins
5. filtrationThe solid was filtered
6. washwashed with 300 ml of water and suck
7. customdried
8. additionThe wet cake and 1500 ml of water were charged into a clean RB and adjusted pH 9.0±0.5 with 50% potassium carbonate solution
9. stirringThe reaction mass was stirred
10. filtrationfiltered
11. washthe solid was washed with 150 ml of water
12. customThe obtained solid was dried under vacuum at 73±2° C.