Hydrochloric Acid → 2-chloro-6-fluoro-4-(1H-pyrazol-3-yl)benzonitrile
반응식
[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]참가 물질
6
실험 절차
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).
후처리
- customReaction mixture
- customThus resulting precipitate
- filtrationwas filtered
- washwashed with water
- customdried in vacuum
출처 및 근거
- ORD 기록
- ord-f5e703e5e5c6441092fcaf1b68f22b0a
- 출처 데이터셋
- uspto-grants-2015_03
- 특허 번호
- US08975254B2
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