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2-Chloro-4,6-dimethyl-3-pyridinecarbonitrile → 4,6-Dimethylnicotinonitrile

HRID 399623
ノート
印刷プレビュー

反応式

HRID 399623 の反応式
Cl[C:2]1[C:7]([C:8]#[N:9])=[C:6]([CH3:10])[CH:5]=[C:4]([CH3:11])[N:3]=1.[Sn]>Cl.O>[C:8]([C:7]1[C:6]([CH3:10])=[CH:5][C:4]([CH3:11])=[N:3][CH:2]=1)#[N:9]
参加物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 2232612-Chloro-4,6-dimethyl-3-pyridinecarbonitrileHCID 5352426Tin atom

生成物 1

HCID 2439174,6-Dimethylnicotinonitrile収率 54%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒

実験手順

23 g of 2-chloro-3-cyano-4,6-dimethylpyridine are dissolved in 185 ml of concentrated hydrochloric acid and 240 ml of water. 25.4 g of tin metal are added and the mixture is brought to 100° C. The reaction is monitored by thin layer chromatography (TLC). When the reaction is complete, the mixture is allowed to return to room temperature and filtered and the filtrate is neutralized using sodium hydroxide solution. The mixture is extracted with methylene chloride and the combined organic phases are washed with saturated aqueous sodium bicarbonate solution and dried over anhydrous magnesium sulphate. The solution is concentrated to give 5-cyano-2,4-dimethyl-pyridine in the form of a yellow precipitate.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. customis brought to 100° C
  2. customto return to room temperature
  3. filtrationfiltered
  4. extractionThe mixture is extracted with methylene chloride
  5. washthe combined organic phases are washed with saturated aqueous sodium bicarbonate solution
  6. dry with materialdried over anhydrous magnesium sulphate
  7. concentrationThe solution is concentrated

出典と根拠

ORDレコード
ord-51804f6f471e4dfb910e9c186bc95b92
出典データセット
uspto-grants-1998_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05821255

反応ノート

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