反应详情

Thionyl chloride (1.72 g, 14.4 mmol) was added to a stirred solution of {1-[4-(pentafluoro-λ6-sulfanyl)phenyl]-1H-tetrazol-5-yl}methanol (Intermediate 44, 3.50 g, 11.6 mmol) in toluene (40 mL), SOCl2 at room temperature. The reaction mixture was stirred for 4 hr at reflux. The reaction mixture was concentrated under vacuum. The residue was diluted with DCM and washed with ice-water, saturated aq NaHCO3 and brine solution, dried over anhydrous Na2SO4, and concentrated under reduced pressure to give the crude compound. This was purified by column chromatography (100-200 mesh silica gel), eluted with 20%-30% EtOAc/pet-ether to give the title compound as a brown gum (3.50 g).

1. temperatureat reflux
2. concentrationThe reaction mixture was concentrated under vacuum
3. additionThe residue was diluted with DCM
4. washwashed with ice-water, saturated aq NaHCO3 and brine solution
5. dry with materialdried over anhydrous Na2SO4
6. concentrationconcentrated under reduced pressure
7. customto give the crude compound
8. customThis was purified by column chromatography (100-200 mesh silica gel)
9. washeluted with 20%-30% EtOAc/pet-ether