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Methanol → Ethyl N-({[3-(4-{[6-(acetyloxy)hexyl]oxy}butyl)phenyl]amino}carbonyl)glycinate

HRID 857090
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HRID 857090 반응식
[C:1]([O:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][O:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([NH2:22])[CH:17]=1)(=[O:3])[CH3:2].[N:23]([CH2:26][C:27]([O:29][CH2:30][CH3:31])=[O:28])=[C:24]=[O:25].CO>C(Cl)Cl>[C:1]([O:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][O:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]1[CH:17]=[C:18]([NH:22][C:24]([NH:23][CH2:26][C:27]([O:29][CH2:30][CH3:31])=[O:28])=[O:25])[CH:19]=[CH:20][CH:21]=1)(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 76283Ethyl isocyanatoacetateHCID 218672196-[4-(3-Aminophenyl)butoxy]hexyl acetate

생성물 1

HCID 21867037Ethyl N-({[3-(4-{[6-(acetyloxy)hexyl]oxy}butyl)phenyl]amino}carbonyl)glycinate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

6-[4-(3-Aminophenyl)butoxy]hexyl acetate (2.84 g) in CH2Cl2 (30 ml) was treated with ethyl isocyanatoacetate (1.2 ml). After 0.75 h the mixture was treated with MeOH (2 ml) and stirred for 0.5 h. The mixture was concentrated, purified on a 10 g silica Bond Elut cartridge eluting with Et2O-petroleum ether(1:1) and then with Et2O to give the title compound (3.33 g) ES+ve 437 (MH)+.

후처리

  1. concentrationThe mixture was concentrated
  2. custompurified on a 10 g silica Bond Elut cartridge
  3. washeluting with Et2O-petroleum ether(1:1)

출처 및 근거

ORD 기록
ord-a19b952348c64046a0a785ab6a618e4c
출처 데이터셋
uspto-grants-2006_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07144908B2

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