m-Chloroperbenzoic acid → 6-Methylpyridine-3-carbonitrile 1-oxide
반응식
[CH3:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][N:3]=1.ClC1C=CC=C(C(OO)=[O:18])C=1>ClCCl>[C:6]([C:5]1[CH:8]=[CH:9][C:2]([CH3:1])=[N+:3]([O-:18])[CH:4]=1)#[N:7]참가 물질
4
실험 절차
A mixture of 6-methylnicotinonitrile (4.15 g) and 3-chloroperbenzoic acid (8.3 g) in dichloromethane (200 ml) was stirred under an argon atomosphere at room temperature for 16h. The dichloromethane was evaporated under reduced pressure and the residue purified by flash column chromatography on silica (K60), using ethyl acetate and then methanol: dichloromethane (1:9 by volume) as eluting solvent to give 5-cyano-2-methylpyridine-1-oxide, mp 133.5°.
후처리
- customThe dichloromethane was evaporated under reduced pressure
- customthe residue purified by flash column chromatography on silica (K60)
- washmethanol: dichloromethane (1:9 by volume) as eluting solvent
출처 및 근거
- ORD 기록
- ord-a78378da87434bf7a8573388e582ea7e
- 출처 데이터셋
- uspto-grants-1991_03
- 특허 번호
- US04999364
반응 노트
불러오는 중…