Triethylamine → HCID 21276268、化合物

HRID 1381625ノート

反応式

HRID 1381625 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH2:12][NH:13][C:14](=[O:22])[CH2:15][CH2:16][CH2:17][CH2:18][C:19]([OH:21])=O)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].C(N(CC)CC)C.ClC(OCC)=O.[C:36]1([NH:42][CH2:43][CH2:44][NH2:45])[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1>ClCCl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH2:12][NH:13][C:14](=[O:22])[CH2:15][CH2:16][CH2:17][CH2:18][C:19]([NH:45][CH2:44][CH2:43][NH:42][C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)=[O:21])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

参加物

6

反応物 4

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 742701,2-Ethanediamine, N1-phenyl-HCID 139357676-[2-(3,4-Dimethoxyphenyl)ethylamino]-6-oxohexanoic acid

生成物 1

HCID 21276268HCID 21276268、化合物収率 65.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

6-[2-(3,4-Dimethoxyphenyl)ethylamino]-6-oxohexanoic acid (6.0 g, 0.019) was dissolved in dry dichloromethane (200 ml) and triethylamine (2.28 g, 0.021 mole), and ethyl chloroformate (1.86 ml, 0.019 mole) added at 0°. After 1 hour at 0° N-phenyl-1,2-ethanediamine (2.64 g, 0.019 mole) was added and the mixture stirred at room temperature for 18 hr. After washing with water and drying (Na2SO4), the reaction mixture was evaporated and the residue recrystallised from ethyl acetate to give the sub title compound (5.3 g) mp 109°-11°.

後処理

  1. washAfter washing with water
  2. dry with materialdrying (Na2SO4)
  3. customthe reaction mixture was evaporated
  4. customthe residue recrystallised from ethyl acetate

出典と根拠

ORDレコード
ord-0c18f38fb8204b2ab159c3f146d83074
出典データセット
uspto-grants-1989_02
特許番号
US04803225

反応ノート

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