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Dicyclohexylcarbodiimide → N-(3,3-dimethoxypropanoyl)-2-methoxy-5-acetoxy-aniline

HRID 1090702
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HRID 1090702 반응식
[CH3:1][O:2][C:3]1[CH:9]=[CH:8][C:7]([O:10][C:11](=[O:13])[CH3:12])=[CH:6][C:4]=1[NH2:5].[CH3:14][O:15][CH:16]([O:21][CH3:22])[CH2:17][C:18](O)=[O:19].C1CCC(N=C=NC2CCCCC2)CC1>C(Cl)Cl>[CH3:14][O:15][CH:16]([O:21][CH3:22])[CH2:17][C:18]([NH:5][C:4]1[CH:6]=[C:7]([O:10][C:11](=[O:13])[CH3:12])[CH:8]=[CH:9][C:3]=1[O:2][CH3:1])=[O:19]
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참가 물질

5

반응물 3

HCID 10868DicyclohexylcarbodiimideHCID 103745043,3-dimethoxypropanoic AcidHCID 156769772-Methoxy-5-acetyloxy-aniline

생성물 1

HCID 10424696N-(3,3-dimethoxypropanoyl)-2-methoxy-5-acetoxy-aniline수율 95%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
5 °C

실험 절차

To a cooled solution (0° C.) of 2-methoxy-5-acetyloxy-aniline (5 g, 0.0276 mole), 3,3-dimethoxy-propanoic acid (5 g, 0.0373 mole) in 75 ml of methylene chloride was added DCC (5.7 g, 0.0276 mole) in 20 ml of methylene chloride. After completion of the addition, the solution was stirred for a further 4 hours. The reaction medium was concentrated to 25 ml, diluted with 200 ml of isopropyl ether, cooled to 5° C. and the resulting precipitate was isolated by filtration, giving N-(3,3-dimethoxypropanoyl)-2-methoxy-5-acetoxy-aniline 7.7 g (Yield=95%).

후처리

  1. additionAfter completion of the addition
  2. concentrationThe reaction medium was concentrated to 25 ml
  3. additiondiluted with 200 ml of isopropyl ether
  4. customthe resulting precipitate was isolated by filtration

출처 및 근거

ORD 기록
ord-a4ffffd22d0044a2b7baacaccbd1ace8
출처 데이터셋
uspto-grants-1992_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05082847

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