Ammonia → 1-(3-fluoro-4-(5-methyl-1H-1,2,4-triazol-1-yl)phenyl)thiourea
反応式
[NH3:1].[F:2][C:3]1[CH:8]=[C:7]([N:9]=[C:10]=[S:11])[CH:6]=[CH:5][C:4]=1[N:12]1[C:16]([CH3:17])=[N:15][CH:14]=[N:13]1>>[F:2][C:3]1[CH:8]=[C:7]([NH:9][C:10]([NH2:1])=[S:11])[CH:6]=[CH:5][C:4]=1[N:12]1[C:16]([CH3:17])=[N:15][CH:14]=[N:13]1参加物
3
実験手順
Step C (4): Methanolic ammonia (1.0 M, 100 mL, 100 mmol) was added to a flask charged with 1-(2-fluoro-4-isothiocyanatophenyl)-5-methyl-1H-1,2,4-triazole (3.18 g, 13.6 mmol) in a ice-water bath. After the addition was complete, the resulting slurry was stirred for 10 min and then allowed to warm to rt. After 24 h, the reaction mixture was concentrated in vacuo. The resulting solid was dried under high vacuum to afford 1-(3-fluoro-4-(5-methyl-1H-1,2,4-triazol-1-yl)phenyl)thiourea (3.21 g, 94% yield) as an off-white solid. LC-MS (M+H)+ 252.1. 1H NMR (500 MHz, DMSO-d6) δ ppm 8.06 (s, 1 H), 7.93 (dd, J=12.8, 2.1 Hz, 1 H), 7.54 (t, J=8.7 Hz, 1 H), 7.37 (dd, J=8.5, 1.8 Hz, 1 H), 2.32 (s, 3 H)