m-Chloroperbenzoic acid → 6-Methylpyridine-3-carbonitrile 1-oxide

HRID 358983

반응식

HRID 358983 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

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 2819956-Methylpyridine-3-carbonitrile

생성물 1

HCID 198186716-Methylpyridine-3-carbonitrile 1-oxide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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

  1. customThe dichloromethane was evaporated under reduced pressure
  2. customthe residue purified by flash column chromatography on silica (K60)
  3. 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

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