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Water → ethyl (Z)-3-[3'-(3-butyl-1-methylureido)biphenyl-4-yl]-2-ethoxyacrylate

HRID 390683
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HRID 390683 반응식
[CH2:1]([O:3]/[C:4](=[CH:10]\[C:11]1[CH:16]=[CH:15][C:14]([C:17]2[CH:22]=[CH:21][CH:20]=[C:19]([N:23]([CH3:36])[C:24]([O:26]C3C=CC([N+]([O-])=O)=CC=3)=O)[CH:18]=2)=[CH:13][CH:12]=1)/[C:5]([O:7][CH2:8][CH3:9])=[O:6])[CH3:2].[CH2:37]([NH2:41])[CH2:38][CH2:39][CH3:40].O>CN(C)C=O>[CH2:37]([NH:41][C:24](=[O:26])[N:23]([C:19]1[CH:18]=[C:17]([C:14]2[CH:15]=[CH:16][C:11](/[CH:10]=[C:4](\[O:3][CH2:1][CH3:2])/[C:5]([O:7][CH2:8][CH3:9])=[O:6])=[CH:12][CH:13]=2)[CH:22]=[CH:21][CH:20]=1)[CH3:36])[CH2:38][CH2:39][CH3:40]
참가 물질실험 절차후처리출처 및 근거반응 노트

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반응물 3

HCID 962WaterHCID 8007ButylamineHCID 86626081ethyl (Z)-2-ethoxy-3-{3'-[methyl(4-nitrophenoxycarbonyl)amino]biphenyl-4-yl}acrylate

생성물 1

HCID 86626117ethyl (Z)-3-[3'-(3-butyl-1-methylureido)biphenyl-4-yl]-2-ethoxyacrylate수율 63%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 1.75 g (3 mmol) of ethyl (Z)-2-ethoxy-3-{3′-[methyl-(4-nitrophenoxycarbonyl)amino]biphenyl-4-yl}acrylate and 0.4 mL (3.7 mmol) of n-butylamine in 20 mL of dimethylformamide is heated at 80° C. for 2 hours. After addition of water, the reaction medium is extracted with ethyl acetate, washed with water, dried over magnesium sulfate, filtered and evaporated. The residue obtained is purified by chromatography on a column of silica eluted with a 70/30 heptane/ethyl acetate mixture. 0.8 g (63%) of ethyl (Z)-3-[3′-(3-butyl-1-methylureido)biphenyl-4-yl]-2-ethoxyacrylate is obtained in the form of a white solid after trituration from pentane.

후처리

  1. extractionthe reaction medium is extracted with ethyl acetate
  2. washwashed with water
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue obtained
  7. customis purified by chromatography on a column of silica
  8. washeluted with a 70/30 heptane/ethyl acetate mixture

출처 및 근거

ORD 기록
ord-04b2bea031844ed297740e7c864ed326
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08383652B2

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