反应详情

To a solution of 6-bromo-7-methyl-8-(3-trifluoromethyl-phenyl)-2H-[1,2,4]triazolo[4,3-a]pyridin-3-one (Int. 15, 55 mg, 0.148 mmol) in DMF (3 mL) was added cesium carbonate (58 mg, 0.177 mmol) followed by 4-(methylsulfonyl)benzyl bromide (40 mg, 0.163 mmol) and the mixture was stirred at RT for 20 hrs. Further amounts of cesium carbonate (25 mg) and 4-(methylsulfonyl)benzyl bromide (20 mg) were added and stirring was continued for 2 hrs. Water was added and the mixture was extracted with EtOAc (2×25 mL). The combined organic extracts were washed with brine then dried (Na2SO4), filtered and evaporated in vacuo. The resultant residue was purified by flash chromatography, eluting with a gradient of 0-100% EtOAc in cyclohexane to give the title compound as a yellow solid (49 mg).

1. stirringstirring
2. waitwas continued for 2 hrs
3. extractionthe mixture was extracted with EtOAc (2×25 mL)
4. washThe combined organic extracts were washed with brine
5. dry with materialthen dried (Na2SO4)
6. filtrationfiltered
7. customevaporated in vacuo
8. customThe resultant residue was purified by flash chromatography
9. washeluting with a gradient of 0-100% EtOAc in cyclohexane