Triethylamine → HCID 20459476、化合物

HRID 544129

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

5

反応物 3

HCID 8471TriethylamineHCID 12648(1-Chloroethyl)benzeneHCID 1103156856655-17-5

生成物 1

HCID 20459476HCID 20459476、化合物

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
特許番号
US04448776

関連ノート

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