Sodium Cyanide → 3-Chloro-5-(trifluoromethyl)pyridine-2-carbonitrile
반응식
[C-:1]#[N:2].[Na+].[Cl:4][C:5]1[C:6](F)=[N:7][CH:8]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:10]=1>O.C(#N)CC.CN(C)C1C=CN=CC=1>[Cl:4][C:5]1[C:6]([C:1]#[N:2])=[N:7][CH:8]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:10]=1참가 물질
6
반응 조건
- 온도
- 20 °C
실험 절차
A reactor was charged with a solution of sodium cyanide (73.5 g) in water (150 ml), propionitrile (500 ml), 4-dimethylaminopyridine (16 g), and 3-chloro-2-fluoro-5-trifluoromethylpyridine (149.3 g) added over 30 minutes. After stirring for 5 hours at 20° C., the upper organic phase was separated off and washed with water. The lower aqueous layer was extracted with propionitrile, the two organic layers combined and solvent distilled off under vacuum at 45° C. to give an 83% yield of 3-chloro-2-cyano-5-trifluoromethylpyridine.
후처리
- additionadded over 30 minutes
- customthe upper organic phase was separated off
- washwashed with water
- extractionThe lower aqueous layer was extracted with propionitrile
- distillationsolvent distilled off under vacuum at 45° C.
출처 및 근거
- ORD 기록
- ord-25f66ee5310c437fb8f594e64e59f8fe
- 출처 데이터셋
- uspto-grants-2004_03
- 특허 번호
- US06699993B1
반응 노트
불러오는 중…