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Water → N,N-dimethyl-1-(2-phenylphenyl)methanamine

HRID 2418799
ノート
印刷プレビュー

反応式

HRID 2418799 の反応式
[CH3:1][N:2]([CH3:17])[C:3]([C:5]1[C:6]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:7][CH:8]=[CH:9][CH:10]=1)=O.[H-].[Al+3].[Li+].[H-].[H-].[H-].O>COCCOC>[CH3:1][N:2]([CH3:17])[CH2:3][C:5]1[C:6]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:7][CH:8]=[CH:9][CH:10]=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 3

HCID 962WaterHCID 976212N,N-Dimethyl(1,1'-biphenyl)-2-carboxamideHCID 21226445Aluminium lithium hydride

生成物 1

HCID 9859729N,N-dimethyl-1-(2-phenylphenyl)methanamine収率 106.9%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

Under a dry nitrogen atmosphere, 6.1 g (0.027 mole) of N,N-dimethyl-[1,1'-biphenyl]-2-carboxamide was dissolved with stirring in 250 ml of dry 1,2-dimethoxyethane. To this solution was added portionwise 1.3 g (0.034 mole) of lithium aluminum hydride. Upon complete addition, the reaction mixture was heated at reflux temperature for 18 hours. The reaction mixture was then cooled to room temperature, and 1.22 ml (0.068 mole) of water was added dropwise. The reaction mixture was filtered, and the filtrate concentrated under reduced pressure to give 6.1 g (100% yield) of N,N-dimethyl-[1,1'-biphenyl]-2-methanamine as a yellow liquid.

後処理

  1. additionUpon complete addition
  2. temperaturethe reaction mixture was heated
  3. temperatureat reflux temperature for 18 hours
  4. filtrationThe reaction mixture was filtered
  5. concentrationthe filtrate concentrated under reduced pressure

出典と根拠

ORDレコード
ord-d806958a46634229bb342e47827a58b5
出典データセット
uspto-grants-1984_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04473709

反応ノート

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