反応式
[F:1][B-](F)(F)F.[Br:6][C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[C:14]([O:17][CH3:18])[N:15]=2)[N:10]=[CH:9][C:8]=1[N+]#N>C1C2C(CCCC2)CCC1.C(Cl)(Cl)Cl>[Br:6][C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[C:14]([O:17][CH3:18])[N:15]=2)[N:10]=[CH:9][C:8]=1[F:1]参加物
4
反応条件
- 温度
- 180 °C
実験手順
A suspension of 4-bromo-6-methoxy-[1,5]naphthyridine-3-diazonium tetrafluoroborate (31.42 g, 89.0 mmol) in decalin (mixed isomers, 500 mL) in a 2 L flask* was heated to 180° C. and held at this temperature for 5 min. The mixture was cooled and diluted with CHCl3 (500 mL, to keep the product in solution), and the resulting mixture was stirred vigorously for 30 min to break up a black solid byproduct. The mixture was then poured onto a column of silica gel and the column was eluted with CHCl3 to remove decalin and then with 3% EtOAc/CHCl3 to afford the title compound (9.16 g, 40%).
後処理
- temperatureThe mixture was cooled
- additionThe mixture was then poured onto a column of silica gel
- washthe column was eluted with CHCl3
- customto remove decalin
出典と根拠
- ORDレコード
- ord-d8ced98fc8c34c459e21c97cff70057e
- 出典データセット
- uspto-grants-2010_04
- 特許番号
- US07691850B2
関連ノート
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