2-Hydrazinyl-3-(trifluoromethyl)pyridine → 4-iodo-1-(3-(trifluoromethyl)pyridin-2-yl)-1H-pyrazolo[3,4-b]pyridine
反応式
[F:1][C:2]([F:12])([F:11])[C:3]1[C:4]([NH:9][NH2:10])=[N:5][CH:6]=[CH:7][CH:8]=1.[I:13][C:14]1[CH:19]=[CH:18][N:17]=[C:16](F)[C:15]=1[CH:21]=O>CN1C(=O)CCC1>[I:13][C:14]1[CH:19]=[CH:18][N:17]=[C:16]2[N:9]([C:4]3[C:3]([C:2]([F:1])([F:11])[F:12])=[CH:8][CH:7]=[CH:6][N:5]=3)[N:10]=[CH:21][C:15]=12参加物
4
反応条件
- 温度
- 185 °C
実験手順
To a dry 15 mL ChemGlass pressure bottle under nitrogen was added 3-(trifluoromethyl)pyrid-2-ylhydrazine (499 mg, 2.82 mmol), 4-iodo-2-fluoro-3-formylpyridine (706.8 mg, 2.82 mmol) and anhydrous NMP (4.5 mL). The reaction mixture was flushed with argon, securely capped and heated to 185° C. for 1.5 h. The reaction mixture was worked up according to the procedure described in Intermediate 69A to give 982 mg (89%) of the title compound as an oil. LC/MS (Condition B): ret. T=3.4 min, (M+H)+ 390.94.