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Triethylamine → N-diphenylmethyl-N'-(1-phenylethyl)-ethylenediamine

HRID 544129
ノート
印刷プレビュー

反応式

HRID 544129 の反応式
[C:1]1([CH:7]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[NH:8][CH2:9][CH2:10][NH2:11])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.[C:25]1([CH:31](Cl)[CH3:32])[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1>C(#N)C>[C:1]1([CH:7]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[NH:8][CH2:9][CH2:10][NH:11][CH:31]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH3:32])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=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 8471TriethylamineHCID 12648(1-Chloroethyl)benzeneHCID 11031568(2-Aminoethyl)(diphenylmethyl)amine

生成物 1

HCID 20459476N-diphenylmethyl-N'-(1-phenylethyl)-ethylenediamine

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

11 g of N-diphenylmethyl-ethylenediamine, 10.1 g of triethylamine and 7.0 g of 1-phenylethyl chloride are dissolved, while stirring, in 85 ml of acetonitrile and heated under reflux for 30 hours. The solution is concentrated by evaporation under reduced pressure, 50 ml of 10% sodium hydroxide solution are added and the mixture is extracted thoroughly by shaking with diethyl ether. The ether extracts are combined, dried over sodium sulphate and concentrated by evaporation. N-diphenylmethyl-N'-(1-phenylethyl)-ethylenediamine is obtained in the form of a yellow oil which can be purified chromatographically over silica gel with methanol/ethyl acetate (1:1) as the eluant and, for characterisation, can be converted into the dihydrochloride, having a melting point of 160° C., as described in Example 4.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 30 hours
  3. concentrationThe solution is concentrated by evaporation under reduced pressure, 50 ml of 10% sodium hydroxide solution
  4. additionare added
  5. extractionthe mixture is extracted thoroughly
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-4d3a78a70eaf4f2a8d12b6bc40eedb27
出典データセット
uspto-grants-1984_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04448776

反応ノート

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