반응식
[Br:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[CH:4][C:3]=1[C:12]1[CH:21]=[CH:20][CH:19]=[C:18]2[C:13]=1[CH:14]=[CH:15][C:16]([S:22]([N:25](CC1C=CC(OC)=CC=1OC)[C:26]1[S:30][N:29]=[CH:28][N:27]=1)(=[O:24])=[O:23])=[CH:17]2.C(Cl)Cl.C(O)(C(F)(F)F)=O>>[Br:1][C:2]1[CH:7]=[C:6]([C:8]([F:10])([F:11])[F:9])[CH:5]=[CH:4][C:3]=1[C:12]1[CH:21]=[CH:20][CH:19]=[C:18]2[C:13]=1[CH:14]=[CH:15][C:16]([S:22]([NH:25][C:26]1[S:30][N:29]=[CH:28][N:27]=1)(=[O:23])=[O:24])=[CH:17]2참가 물질
실험 절차
To a solution of 5-(2-bromo-4-(trifluoromethyl)phenyl)-N-(2,4-dimethoxybenzyl)-N-(1,2,4-thiadiazol-5-yl)naphthalene-2-sulfonamide (3.27 g, 4.92 mmol) in DCM (49.2 mL, 4.92 mmol) was added TFA (1.896 mL, 24.60 mmol). The resulting mixture was stirred at room temperature. After 30 min, LC/MS showed mainly desired product. The mixture was stirred for an additional hour at room temperature until the reaction was complete. The mixture was partially concentrated until a white solid crashed out. The solid was filtered, washed with diethyl ether and dried to afford 5-(2-bromo-4-(trifluoromethyl)phenyl)-N-(1,2,4-thiadiazol-5-yl)naphthalene-2-sulfonamide (2.4 g, 4.67 mmol). 1H NMR (500 MHz, DMSO-d6) δ ppm 7.58 (d, J=8.76 Hz, 1H) 7.68-7.74 (m, 1H) 7.74-7.83 (m, 2H) 7.87 (d, J=8.01 Hz, 1H) 8.16-8.24 (m, 2H) 8.34 (d, J=8.34 Hz, 1H) 8.52-8.57 (m, 2H); m/z (ESI) 513.7 (M+H)+.
출처 및 근거
- ORD 기록
- ord-f217003fd2bb4baf80d0b1a9e58f2860
- 출처 데이터셋
- uspto-grants-2015_04
- 특허 번호
- US09012443B2
연결된 노트
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