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Benzylamine → N-benzyl-3,5,6-trifluoropyridin-2-amine

HRID 1274662
ノート
印刷プレビュー

反応式

HRID 1274662 の反応式
F[C:2]1[C:7]([F:8])=[CH:6][C:5]([F:9])=[C:4]([F:10])[N:3]=1.[CH2:11]([NH2:18])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>C(#N)C>[CH2:11]([NH:18][C:2]1[C:7]([F:8])=[CH:6][C:5]([F:9])=[C:4]([F:10])[N:3]=1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 7504BenzylamineHCID 1377492,3,5,6-Tetrafluoropyridine

生成物 1

HCID 22121263N-benzyl-3,5,6-trifluoropyridin-2-amine収率 84.6%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To 50 ml of acetonitrile were added 12.0 g of 2,3,5,6-tetrafluoropyridine and 18.0 g of benzylamine, and the mixture was stirred under reflux condition for 2 hours, and the solvent and the like were distilled off. To the residue was added 150 ml of ethyl acetate, and the mixture was washed twice with 150 ml of distilled water and 150 ml of 10% aqueous solution of citric acid. The ethyl acetate layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 16.0 g of the title compound as a pale yellow oil.

後処理

  1. temperatureunder reflux condition for 2 hours
  2. distillationthe solvent and the like were distilled off
  3. additionTo the residue was added 150 ml of ethyl acetate
  4. washthe mixture was washed twice with 150 ml of distilled water and 150 ml of 10% aqueous solution of citric acid
  5. dry with materialThe ethyl acetate layer was dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-4f7edaf7fa4e46d4b84306668461a03e
出典データセット
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06156903

反応ノート

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