Diethyl Ether → ([1,1'-Biphenyl]-2-yl)-N,N,N-trimethylmethanaminium iodide

HRID 2418800ノート

反応式

HRID 2418800 の反応式
[CH3:1][N:2]([CH3:16])[CH2:3][C:4]1[C:5]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:6][CH:7]=[CH:8][CH:9]=1.C[I:18].[CH2:19](OCC)C>C(O)C>[I-:18].[CH3:1][N+:2]([CH3:19])([CH3:16])[CH2:3][C:4]1[C:5]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:6][CH:7]=[CH:8][CH:9]=1

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 6328Methyl iodideHCID 9859729N,N-dimethyl-1-(2-phenylphenyl)methanamine

生成物 1

HCID 13374112([1,1'-Biphenyl]-2-yl)-N,N,N-trimethylmethanaminium iodide収率 100%

試薬・触媒・溶媒 1

HCID 702Ethanol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-methanamine was dissolved with stirring in 6.4 ml of anhydrous ethanol. To this solution 5.1 g (0.036 mole) of methyl iodide was added slowly. After complete addition, the reaction mixture was heated at reflux temperature for 45 minutes, then cooled. Diethyl ether was added until the mixture was cloudy, then the whole was placed in a freezer for 16 hours. An oil which had formed in the mixture was separated then dissolved in ethanol, and the solution was concentrated under reduced pressure to give 10.0 g (100% yield) of N,N,N-trimethyl-[1,1'-biphenyl]-2-methanaminium iodide as a brittle yellow foam.

後処理

  1. additionAfter complete addition
  2. temperaturethe reaction mixture was heated
  3. temperatureat reflux temperature for 45 minutes
  4. temperaturecooled
  5. customAn oil which had formed in the mixture
  6. customwas separated
  7. dissolutionthen dissolved in ethanol
  8. concentrationthe solution was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-0acac3871242481eba2ac290e776a2e4
出典データセット
uspto-grants-1984_09
特許番号
US04473709

反応ノート

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