反应详情

温度

23 °C

To a suspension of 3-[6′-methyl-4′-(4-trifluoromethyl-phenyl)-[2,2′]bipyridinyl-6-yl]-benzenesulfonic acid (example 345) (2.0 g, 4.25 mmol) in DMF (20 mL) at 23° C. was added thionyl chloride (1.54 mL, 21.25 mmol) and the mixture was stirred at 23° C. for 2 h, then added again SOCl2 (1.54 mL, 21.25 mmol) and the mixture was stirred at 23° C. for 1 h. Diluted with EtOAc, poured into ice cold half-sat. NaHCO3-sol., separated phases, washed organic layer with brine and dried over Na2SO4. Removal of the solvent in vacuum left the title compound as an off-white solid (2.0 g, 98%), which was used without further purification. MS (ISP) 489.2 [(M+H)+] and 491.1 [(M+2+H)+].

1. stirringthe mixture was stirred at 23° C. for 1 h
2. custom, separated phases
3. washwashed organic layer with brine
4. dry with materialdried over Na2SO4
5. customRemoval of the solvent in vacuum
6. waitleft the title compound as an off-white solid (2.0 g, 98%), which
7. customwas used without further purification