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Water → ethyl (Z)-2-ethoxy-3-{3'-[methyl(4-nitrophenoxycarbonyl)amino]biphenyl-4-yl}acrylate

HRID 390678
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HRID 390678 반응식
Cl[C:2]([O:4][C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][CH:6]=1)=[O:3].C(NCC)C.[CH2:19]([O:21]/[C:22](=[CH:28]\[C:29]1[CH:34]=[CH:33][C:32]([C:35]2[CH:40]=[CH:39][CH:38]=[C:37]([NH:41][CH3:42])[CH:36]=2)=[CH:31][CH:30]=1)/[C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH3:20].O>ClCCl>[CH2:19]([O:21]/[C:22](=[CH:28]\[C:29]1[CH:34]=[CH:33][C:32]([C:35]2[CH:40]=[CH:39][CH:38]=[C:37]([N:41]([CH3:42])[C:2]([O:4][C:5]3[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][CH:6]=3)=[O:3])[CH:36]=2)=[CH:31][CH:30]=1)/[C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH3:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 8021DiethylamineHCID 821294-Nitrophenyl chloroformateHCID 86626079ethyl (Z)-2-ethoxy-3-(3'-methylaminobiphenyl-4-yl)acrylate

생성물 1

HCID 86626081ethyl (Z)-2-ethoxy-3-{3'-[methyl(4-nitrophenoxycarbonyl)amino]biphenyl-4-yl}acrylate수율 126.2%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

0.63 g (3.1 mmol) of 4-nitrophenyl chloroformate and then 0.54 mL (3.1 mmol) of diethylamine are added to a solution of 0.68 g (2.1 mmol) of ethyl (Z)-2-ethoxy-3-(3′-methylaminobiphenyl-4-yl)acrylate in 15 mL of dichloromethane. The reaction mixture is stirred for 1 hour 30 minutes at room temperature. The reaction is worked up by addition of 10 mL of water and then extracted with dichloromethane. The organic phases are combined and then dried over magnesium sulfate. The solvents are evaporated off. 1.3 g (100%) of ethyl (Z)-2-ethoxy-3-{3′-[methyl-(4-nitrophenoxycarbonyl)amino]biphenyl-4-yl}acrylate are obtained in the form of a yellow oil.

후처리

  1. extractionextracted with dichloromethane
  2. dry with materialdried over magnesium sulfate
  3. customThe solvents are evaporated off

출처 및 근거

ORD 기록
ord-fa17fca0c2414bec984c3b6134d3eb22
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08383652B2

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