Nitronium tetrafluoroborate → HCID 21084113、化合物
反応式
[Br:1][C:2]1[N:7]2[N:8]=[C:9]([CH3:11])[CH:10]=[C:6]2[CH:5]=[CH:4][CH:3]=1.F[B-](F)(F)F.[O:17]=[N+:18]=[O:19]>C(#N)C>[Br:1][C:2]1[N:7]2[N:8]=[C:9]([CH3:11])[C:10]([N+:18]([O-:19])=[O:17])=[C:6]2[CH:5]=[CH:4][CH:3]=1参加物
4
実験手順
To a solution of 7-bromo-2-methylpyrazolo[1,5-a]pyridine (1.3 g) dissolved in acetonitrile (25 mL) was added nitronium tetrafluoroborate (900 mg) while stirring on ice, and the reaction mixture was stirred for 10 minutes. The obtained reaction mixture was added to ice water, and the precipitated crystals were collected by filtration, washed with water and then dried under reduced pressure to afford crude crystals. These were purified by silica gel column chromatography and the title compound (900 mg) was obtained as yellow crystals from the n-hexane:ethyl acetate (5:1) fraction.
後処理
- stirringthe reaction mixture was stirred for 10 minutes
- customThe obtained reaction mixture
- filtrationthe precipitated crystals were collected by filtration
- washwashed with water
- customdried under reduced pressure
- customto afford crude crystals
- customThese were purified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-8f258cb84bf54e54b7f4f4715806f635
- 出典データセット
- uspto-grants-2007_02
- 特許番号
- US07176216B2
反応ノート
読み込み中…