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Formamide, N-(1,1'-biphenyl)-4-yl- → 4-Biphenylamine, N-methyl-

HRID 1665679
ノート
印刷プレビュー

反応式

HRID 1665679 の反応式
[H-].[H-].[H-].[H-].[Li+].[Al+3].[C:7]1([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:12]=[CH:11][C:10]([NH:13][CH:14]=O)=[CH:9][CH:8]=1>C1COCC1.C(OCC)(=O)C>[C:7]1([C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH:8]=[CH:9][C:10]([NH:13][CH3:14])=[CH:11][CH:12]=1
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 95684Formamide, N-(1,1'-biphenyl)-4-yl-HCID 21226445Aluminium lithium hydride

生成物 1

HCID 1231884-Biphenylamine, N-methyl-収率 92.8%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

LAH (96 mg, 2.5 mmol) was added portionwise to a cold (at 0° C.) solution of N-biphenyl-4-yl-formamide (100 mg, 0.5 mmol) in THF (2 mL) and the stirring was continued at the same temperature for 30 minutes. After completion of the reaction, the reaction mixture was quenched with 3% aq NaOH solution, the precipitate obtained was filtered, the filtrate was collected was concentrated under reduced pressure to get a residue. The residue was diluted with ethyl acetate, the organic layer was washed with brine solution and dried over sodium sulfate. The organic layer was concentrated under reduced pressure to afford 85 mg (91.39% Yield) of biphenyl-4-yl-methyl-amine.

後処理

  1. customAfter completion of the reaction
  2. customthe reaction mixture was quenched with 3% aq NaOH solution
  3. customthe precipitate obtained
  4. filtrationwas filtered
  5. customthe filtrate was collected
  6. concentrationwas concentrated under reduced pressure
  7. customto get a residue
  8. washthe organic layer was washed with brine solution
  9. dry with materialdried over sodium sulfate
  10. concentrationThe organic layer was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-d1e4b563dbf24f99805fdff2f11b46cf
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08039463B2

反応ノート

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