Hydrochloric Acid → 2-chloro-6-fluoro-4-(1H-pyrazol-3-yl)benzonitrile
反応式
[Cl:1][C:2]1[CH:9]=[C:8]([C:10]2[N:14](C3CCCCO3)[N:13]=[CH:12][CH:11]=2)[CH:7]=[C:6]([F:21])[C:3]=1[C:4]#[N:5].Cl.CCO.C([O-])(O)=O.[Na+]>O>[Cl:1][C:2]1[CH:9]=[C:8]([C:10]2[NH:14][N:13]=[CH:12][CH:11]=2)[CH:7]=[C:6]([F:21])[C:3]=1[C:4]#[N:5]参加物
6
実験手順
2-Chloro-6-fluoro-4-(1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-5-yl)benzonitrile (1.09 g, 3.55 mmol) was stirred with 10% HCl (g)/EtOH-solution (50 ml) at room temperature for 1 h. Reaction mixture was poured into water (50 ml) and made slightly alkaline with saturated NaHCO3 solution. Thus resulting precipitate was filtered, washed with water and dried in vacuum to obtain 0.74 g (94%) of the title compound. 1H-NMR (400 MHz; d6-DMSO): δ 7.06 (d, 1H), 7.94 (dd, 1H), 8.05 (m, 1H), 13.4 (bs, 1H).
後処理
- customReaction mixture
- customThus resulting precipitate
- filtrationwas filtered
- washwashed with water
- customdried in vacuum
出典と根拠
- ORDレコード
- ord-f5e703e5e5c6441092fcaf1b68f22b0a
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08975254B2
反応ノート
読み込み中…