Methyl Acrylate → 4-Cyano-4-(4-methoxy-dibenzofuran-1-yl)-heptane dioic acid dimethyl ester

HRID 2383974

반응식

HRID 2383974 반응식
[CH3:1][O:2][C:3]1[C:8]2[O:9][C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=3[C:7]=2[C:6]([CH2:16][C:17]#[N:18])=[CH:5][CH:4]=1.[C:19]([O:23][CH3:24])(=[O:22])[CH:20]=[CH2:21]>C(#N)C.C(OCC)(=O)C>[CH3:24][O:23][C:19](=[O:22])[CH2:20][CH2:21][C:16]([C:17]#[N:18])([C:6]1[C:7]2[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[O:9][C:8]=2[C:3]([O:2][CH3:1])=[CH:4][CH:5]=1)[CH2:21][CH2:20][C:19]([O:23][CH3:24])=[O:22]

참가 물질

5

반응물 2

HCID 7294Methyl AcrylateHCID 57431693(4-Methoxy-dibenzofuran-1-yl)-acetonitrile

생성물 1

HCID 866358264-Cyano-4-(4-methoxy-dibenzofuran-1-yl)-heptane dioic acid dimethyl ester

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 8857Ethyl Acetate용매

반응 조건

온도
90 °C

실험 절차

To a solution of (4-methoxy-dibenzofuran-1-yl)-acetonitrile (7 g, 0.029 mol) in acetonitrile (200 ml), Triton B (2.7 ml, 0.0147 mol) was added under N2 at RT. The reaction mass was heated to reflux and at reflux temperature methyl acrylate (28.25 ml, 0.295 mol) was added drop wise. The reaction mass was stirred for 4 hrs at 90° C. Once the product is formed, the reaction mass was diluted with ethyl acetate and concentrated under vacuum. 4-cyano-4-(4-methoxy-dibenzofuran-1-yl)-heptane dioic acid dimethyl ester was isolated by column chromatography. Yield 8 g (65%)

후처리

  1. temperatureThe reaction mass was heated
  2. temperatureto reflux
  3. additionwas added drop wise
  4. customOnce the product is formed
  5. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-3f01271ada97438894fb4a32eda6e978
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08263648B2

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