Dimethylformamide dimethyl acetal → 4-((1E)-2-(Dimethylamino)ethenyl)-3-pyridinecarbonitrile

HRID 1049382

反応式

HRID 1049382 の反応式
[CH3:1][N:2]([CH:4](OC)OC)[CH3:3].[CH3:9][C:10]1[C:15]([C:16]#[N:17])=[CH:14][N:13]=[CH:12][CH:11]=1>CN(C=O)C>[CH3:1][N:2]([CH3:3])/[CH:4]=[CH:9]/[C:10]1[C:15]([C:16]#[N:17])=[CH:14][N:13]=[CH:12][CH:11]=1

参加物

4

反応物 2

HCID 78373Dimethylformamide dimethyl acetalHCID 2278064-Methyl-3-cyanopyridine

生成物 1

HCID 124604474-((1E)-2-(Dimethylamino)ethenyl)-3-pyridinecarbonitrile

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
35 °C

実験手順

940 ml of DMF dimethyl acetal are added to a solution of 200 g of 4-methylnicotinonitrile in 940 g of DMF, and the mixture is heated under reflux at 120-110 for 3 days. The mixture is cooled to 35° C., poured into 10 liters of ice-water and cooled at 4° C. for 16 h. The precipitate is filtered off, washed with water and dried, giving 263 g of 4-((E)-2-dimethylaminovinyl)nicotinonitrile; M˜173.22 g/mol; M+H found 174, NMR corresponds.

後処理

  1. temperaturethe mixture is heated
  2. temperatureunder reflux at 120-110 for 3 days
  3. temperaturecooled at 4° C. for 16 h
  4. filtrationThe precipitate is filtered off
  5. washwashed with water
  6. customdried

出典と根拠

ORDレコード
ord-9c93a404358743598e18c0b4a190c824
出典データセット
uspto-grants-2016_07
特許番号
US09382244B2

関連ノート

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