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Dimethylformamide → 5-Chloro-4-(trifluoromethyl)-2-pyridinecarbonitrile

HRID 1880723
ノート
印刷プレビュー

反応式

HRID 1880723 の反応式
[CH3:1][N:2](C)C=O.Cl[C:7]1[CH:12]=[C:11]([C:13]([F:16])([F:15])[F:14])[C:10]([Cl:17])=[CH:9][N:8]=1>[C-]#N.[Zn+2].[C-]#N.O>[Cl:17][C:10]1[C:11]([C:13]([F:16])([F:15])[F:14])=[CH:12][C:7]([C:1]#[N:2])=[N:8][CH:9]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 6228DimethylformamideHCID 269860162,5-Dichloro-4-(trifluoromethyl)pyridine

生成物 1

HCID 595703895-Chloro-4-(trifluoromethyl)-2-pyridinecarbonitrile

試薬・触媒・溶媒 2

HCID 11186Zinc cyanide (Zn(CN)2)触媒HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

To 14 ml of N,N-dimethylformamide were added 1 g of 2,5-dichloro-4-trifluoromethylpyridine, 1.71 g of zinc cyanide and 0.34 g of tetrakistriphenylphosphine palladium, and the mixture was stirred at 90° C. for 10 hours. After allowing to cool, the reaction solution was poured into water, and the resultant solution was extracted with diethyl ether three times, washed with an aqueous saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.7 g of 5-chloro-4-trifluoromethylpyridine-2-carbonitrile.

後処理

  1. temperatureto cool
  2. extractionthe resultant solution was extracted with diethyl ether three times
  3. washwashed with an aqueous saturated sodium chloride solution
  4. dry with materialdried with anhydrous magnesium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-ec1490629a9241e5b950aa754544d600
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08318776B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート