반응 #9213
ord-871ba8cd3b864435860dd69669537659
반응 방정식
1-(6-bromo-7-hydroxy-2-benzothiazolyl)-3-ethyl-urea
(CF3SO2)2O
→
1-(6-Bromo-7-trifluoromethanesulfonyl-2-benzthiazolyl)-3-ethyl-urea
용매
반응 조건
온도
35°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타The solvent was then evaporated
- 2기타The crude material was purified by LC/MS
- 3기타to give 23 mg (32%) pure 14
실험 절차
To a solution of 1-(6-bromo-7-hydroxy-2-benzothiazolyl)-3-ethyl-urea (50 mg, 0.158 mmol) in pyridine (1 mL) were added 3 portions of (CF3SO2)2O (29 μL, 0.174 mmol) about 45 minutes apart. The reaction mixture was stirred for about 3 hours at about 35° C. The solvent was then evaporated. The crude material was purified by LC/MS to give 23 mg (32%) pure 14. 1H NMR (DMSO) δ 1.09 (t, 3H, J=8 Hz CH3), 3.19 (m, 2H, CH2), 6.79 (br s, 1H, NH), 7.67 (d, 1H, J=12 Hz, ArH), 7.80 (d, 1H, J=8 Hz, ArH), 11.20 (br s, 1H, NH). HPLC retention time 3.58 minutes.