반응 #2028879
ord-cbe117f1f0da4e85b1f0a6af291a035e
반응 방정식
alcohol
4-[3-hydroxymethyl-5-phenyl-1H-pyrazol-1-yl]benzene Sulfonamide
diethylaminosulfur trifluoride
→
4-[3-fluoromethyl-5-phenyl-1H-pyrazol-1-yl]benzenesulfonamide
반응물
시약
없음
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타partitioned between water and dichloromethane
- 2세척The organic solution was washed with brine
- 3농축concentrated
- 4기타The residue was chromatographed on silica (72 mg, 34%)
실험 절차
To a mixture of the alcohol from Step 3 (212 mg, 0.64 mmol) in dichloromethane (4 mL) was added diethylaminosulfur trifluoride (0.13 mL, 1.0 mmol). The reaction mixture was stirred at room temperature for 3 hours and partitioned between water and dichloromethane. The organic solution was washed with brine and concentrated. The residue was chromatographed on silica (72 mg, 34%): mp 162°-163° C.; Anal. calc'd for C16H14N3O2SF: C, 58.00; H, 4.26; N, 12.68. Found: C, 57.95; H, 4.03; N, 12.58.