2-Aminophenol → 867353-53-5

HRID 2354140ノート

反応式

HRID 2354140 の反応式
[C:1]([O:5][C:6]([NH:8][CH2:9][CH2:10][C:11]([OH:13])=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].[NH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[OH:21].C1(N=C=NC2CCCCC2)CCCCC1>ClCCl>[C:1]([O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][C:11](=[O:13])[NH:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[OH:21])([CH3:2])([CH3:3])[CH3:4]

参加物

5

反応物 3

HCID 58012-AminophenolHCID 10868DicyclohexylcarbodiimideHCID 76809N-((1,1-dimethylethoxy)carbonyl)-beta-alanine

生成物 1

HCID 51284468867353-53-5

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a suspension of 3-tert-Butoxycarbonylamino-propionic acid (5-1) (1.0 g, 5.3 mmol) and 2-aminophenol (5-2) (578 mg, 5.3 mmol) in dichloromethane (10 mL) was added N,N′-dicyclo hexyl carbodiimide (1.3 g, 6.4 mmol). The resulting mixture was stirred at room temperature overnight. The volatile solvents were removed by rotovap evaporation then the reaction mixture was directly purified by silica gel chromatography (10-100% Hexane/Ethyl Acetate) to recover the desired product (5-3) as white solid: 1H-NMR (500 MHz, d4-CD3OD) δ7.43 (m, 1H), 6.88 (m, 1H), 6.76 (m, 1H), 6.70 (m, 1H), 3.29 (m, 2H), 2.48 (m, 2H), 1.29 (s, 9H).

後処理

  1. customThe volatile solvents were removed by rotovap evaporation
  2. customthe reaction mixture was directly purified by silica gel chromatography (10-100% Hexane/Ethyl Acetate)
  3. customto recover the desired product (5-3) as white solid

出典と根拠

ORDレコード
ord-f3dfb09129fc459fa6c9223fc23796ab
出典データセット
uspto-grants-2010_07
特許番号
US07750151B2

反応ノート

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