N,N'-Dicyclohexylurea → 3-Dimethylamino-1,1-diphenyl-propan-2-ol

HRID 866948ノート

反応式

HRID 866948 の反応式
[CH3:1][N:2]([CH3:19])[CH2:3][CH:4]([OH:18])[CH:5]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.Cl.[CH2:21]([N:23]([CH2:30][CH3:31])[CH2:24][CH2:25][CH2:26][C:27]([OH:29])=[O:28])[CH3:22].C1(N=C=NC2CCCCC2)CCCCC1.C(NC1CCCCC1)(NC1CCCCC1)=O>ClCCl>[CH2:30]([N:23]([CH2:21][CH3:22])[CH2:24][CH2:25][CH2:26][C:27]([O-:29])=[O:28])[CH3:31].[CH3:19][N:2]([CH3:1])[CH2:3][CH:4]([OH:18])[CH:5]([C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1

参加物

7

反応物 4

HCID 4277N,N'-DicyclohexylureaHCID 10868DicyclohexylcarbodiimideHCID 125491223-Dimethylamino-1,1-diphenyl-propan-2-olHCID 137955394-(Diethylamino)butanoic acid hydrochloride

生成物 2

HCID 125491223-Dimethylamino-1,1-diphenyl-propan-2-olHCID 203090674-Diethylaminobutyrate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 3-dimethylamino-1,1-diphenyl-propan-2-ol (2 55g) 4-diethylaminobutyric acid hydrochloride (1 95g.) and dicyclohexylcarbodiimide (2.1g.) in dichloromethane (50 ml) was stirred at room temperature for 5 days Dicyclohexylurea was filtered off and the filtrate concentrated. The residue was dissolved in dilute hydrochloric acid and ether. The acid extract was basified; isolation through ether in the normal manner gave an oil which was chromatographed as alumina (200g.). Elution with progressively graded mixtures of light petroleum and ether gave the 4-diethylaminobutyrate of 3-dimethylamino-1,1-diphenyl-propan-2-ol isolated as the dihydrochloride (41%) as a glass

後処理

  1. filtrationwas filtered off
  2. concentrationthe filtrate concentrated
  3. dissolutionThe residue was dissolved in dilute hydrochloric acid
  4. extractionThe acid extract
  5. customisolation through ether in the normal manner gave an oil which
  6. customwas chromatographed as alumina (200g.)
  7. washElution with progressively graded mixtures of light petroleum and ether

出典と根拠

ORDレコード
ord-8a6e4c9499d947fca1c78b36b1648311
出典データセット
uspto-grants-1978_07
特許番号
US04101676

反応ノート

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