反应详情

温度

25 °C

N-(2,6-difluorophenyl)-5-methyl-1,2,4-triazole-3-sulphonamide (5 g) (Compound A81) was added in portions to a suspension of sodium hydride (1.37 g in 80% suspension in oil) in dry dimethylformamide (40 ml). The mixture was stirred for 30 minutes at 25° C., 4,6-dimethyl-2-chloropyrimidine (2.6 g) was added, and the mixture was then stirred at 100° C. for 18 hours. The cooled reaction mixture was poured into water, acidified with glacial acetic acid and then extracted with dichloromethane (3×100 ml). The organic phases were dried and evaporated, and the residue was chromatographed (silica/dichloromethane). The product was recrystallised from ethanol to give 0.8 g of the desired product, mp 228°-230° C., identical to that of Example A63.

1. stirringthe mixture was then stirred at 100° C. for 18 hours
2. customThe cooled reaction mixture
3. extractionextracted with dichloromethane (3×100 ml)
4. customThe organic phases were dried
5. customevaporated
6. customthe residue was chromatographed (silica/dichloromethane)
7. customThe product was recrystallised from ethanol