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

HRID 2383974

反応式

HRID 2383974 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
90 °C

実験手順

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%)

後処理

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

出典と根拠

ORDレコード
ord-3f01271ada97438894fb4a32eda6e978
出典データセット
uspto-grants-2012_09
特許番号
US08263648B2

関連ノート

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