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Dimethylformamide → 3-[2-(Dimethylamino)ethenyl]pyridine-2-carbonitrile

HRID 47063
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인쇄 미리보기

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HRID 47063 반응식
[CH3:1][C:2]1[C:3]([C:8]#[N:9])=[N:4][CH:5]=[CH:6][CH:7]=1.[CH3:10][N:11]([CH:13]=O)[CH3:12]>>[CH3:10][N:11]([CH3:13])[CH:12]=[CH:1][C:2]1[C:3]([C:8]#[N:9])=[N:4][CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 6228DimethylformamideHCID 8199283-Methylpyridine-2-carbonitrile

생성물 1

HCID 537133073-[2-(Dimethylamino)ethenyl]pyridine-2-carbonitrile수율 56%

실험 절차

A solution of 3-methyl-2-cyanopyridine (20.0 g, 0.17 m), DMF (200 mL) and DMF acetal (30 mL, 0.25 m) was heated at 120° with stirring under N2 for 5 days. Additional acetal was periodically added in 5 mL aliquots (total 45 mL, 0.38 m). The solution was then evaporated to dryness to give a crude oil which solidified on standing. The solid was crystallized from ligroin to yield 16.5 g (56%) of N,N-dimethyl-2-(2-cyano-3-pyridyl)ethenamine. An analytical sample was prepared by recrystallization from ligroin, mp 71.5°-72°.

후처리

  1. customThe solution was then evaporated to dryness
  2. customto give a crude oil which
  3. customThe solid was crystallized from ligroin

출처 및 근거

ORD 기록
ord-9b7b082db0304f9b872f64baf33f2cfb
출처 데이터셋
uspto-grants-1979_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04176183

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