反应详情

2-Amino-5,8-dimethoxy[1,2,4]triazolo[1,5-c]pyrimidine (7.8 g, 0.040 mol) and 2-(2,2-difluoroethoxy)-6-(trifluoromethyl)benzenesulfonyl chloride (13 g, 0.040 mol) were combined in 3,5-lutidine (31 g, 0.29 mol). The slurry was treated with DMSO (0.040 g, 0.012 eq) and stirred at ambient conditions for 8.5 hours, with a slight rise in temperature noted in the first hours resulting from a reaction exotherm. The reaction slurry was filtered, and the wet cake solids were transferred to a separate vessel and slurried in a mixture of 15% sulfuric acid (80 mL) and acetonitrile (20 mL). The mixture was stirred for 25 minutes, then filtered and the solids washed with water. After drying under vacuum at 55° C., 18 g of product was obtained as a white solid assaying at 97 wt % (90% yield).

1. customresulting from a reaction exotherm
2. filtrationThe reaction slurry was filtered
3. customthe wet cake solids were transferred to a separate vessel
4. additionslurried in a mixture of 15% sulfuric acid (80 mL) and acetonitrile (20 mL)
5. stirringThe mixture was stirred for 25 minutes
6. filtrationfiltered
7. washthe solids washed with water
8. customAfter drying under vacuum at 55° C.