反应详情

温度

130 °C

A mixture of 3-[6′-methyl-4′-(4-trifluoromethyl-phenyl)-[2,2′]bipyridinyl-6-yl]-benzenesulfonamide (example 266) (300 mg, 0.639 mmol) and acetic anhydride (2.42 mL, 25.6 mmol) in acetic acid (5 mL) was stirred at 130° C. for 3 days. Cooled to rt, diluted with EtOAc, extracted with sat. NaHCO3-sol., dried over Na2SO4, filtered off and evaporated totally to give a crude product, which was purified by silica gel column chromatography with n-heptane/ethyl acetate followed by trituration with diethyl ether/n-heptane to give the title compound (290 mg, 88%) as a white solid. MS (ISP) 512.0 [(M+H)+]; mp 244° C.

1. temperatureCooled to rt
2. extractionextracted with sat. NaHCO3-sol
3. dry with material, dried over Na2SO4
4. filtrationfiltered off
5. customevaporated totally
6. customto give a crude product, which
7. customwas purified by silica gel column chromatography with n-heptane/ethyl acetate