反应详情

A solution of protected sulfonamide from step 2 (500 mg, 1 mmol) in a solution of 3 N HCl (5 ml) in EtOH (4 ml) was heated to reflux for 1 hour, cooled and diluted with water (20 ml). The resulting mixture was extracted with methylene chloride, dried (Na2SO4) and the solvent was evaporated. The residue was recrystallized from toluene containing a small amount of ethyl acetate to give the title product (150 mg, 40%): m.p. 259-260° C. Anal. Calc'd. for C16H11N3O2F4S: C, 49.87; H, 2.88; N, 10.90; S, 8.32. Found: C, 50.30; H, 3.10; N, 10.55; S, 8.73.

1. temperatureto reflux for 1 hour
2. temperaturecooled
3. extractionThe resulting mixture was extracted with methylene chloride
4. dry with materialdried (Na2SO4)
5. customthe solvent was evaporated
6. customThe residue was recrystallized from toluene containing a small amount of ethyl acetate