2-Aminophenol → 867353-53-5

HRID 2354140노트

반응식

HRID 2354140 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 51284468867353-53-5

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-f3dfb09129fc459fa6c9223fc23796ab
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07750151B2

반응 노트

불러오는 중…