反应详情

A cooled (0° C.) solution of 6-chloropyrimidine-4-carbonyl chloride (4.56 g; 25.8 mmol) in DCM (80 ml) was treated dropwise over 30 minutes with a solution of 4-amino-3-methyl-benzenesulfonamide (4.00 g; 21.5 mmol) and DIEA (7.40 ml; 43.0 mmol) in anhydrous DMF (10 mL). At the end of addition the reaction mixture was concentrated under vacuum and the residue was taken up in EtOAc (200 mL). The organic phase was washed with water/brine (80 mL). A precipitate was formed, which was filtered and dried under vacuum to afford the crude product which was recrystallized from EtOH. The title product was obtained as a white solid.

1. additionAt the end of addition the reaction mixture
2. concentrationwas concentrated under vacuum
3. washThe organic phase was washed with water/brine (80 mL)
4. customA precipitate was formed
5. filtrationwhich was filtered
6. customdried under vacuum
7. customto afford the crude product which
8. customwas recrystallized from EtOH