4-[But-3-enyl-(2,4-dimethoxybenzyl)-carbamoyl]-pent-4-enoic acid methyl ester → HCID 16720333、化合物

HRID 2240594ノート

反応式

HRID 2240594 の反応式
[CH3:1][O:2][C:3](=[O:26])[CH2:4][CH2:5][C:6]([C:8](=[O:25])[N:9]([CH2:21][CH2:22][CH:23]=C)[CH2:10][C:11]1[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][C:12]=1[O:19][CH3:20])=C>C(Cl)Cl.[Ru]>[CH3:1][O:2][C:3](=[O:26])[CH2:4][CH2:5][C:6]1[C:8](=[O:25])[N:9]([CH2:10][C:11]2[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][C:12]=2[O:19][CH3:20])[CH2:21][CH2:22][CH:23]=1

参加物

4

反応物 1

HCID 167203324-[But-3-enyl-(2,4-dimethoxybenzyl)-carbamoyl]-pent-4-enoic acid methyl ester

生成物 1

HCID 16720333HCID 16720333、化合物収率 90.1%

試薬・触媒・溶媒 2

HCID 23950Ruthenium触媒HCID 6344Dichloromethane溶媒

実験手順

130 mg of the compound (c) (0.360 mM) prepared by the above Step 2 was added to the catalyst solution containing 20 mg of ruthenium (0.024 mM) dissolved in CH2Cl2. Then the mixture was stirred for 24 hrs at room temperature, filtered and concentrated in vacuo. The resultant was purified by Silica gel column chromatography with methanol/chloroform (1:10) solvent mixture as an eluant to give 108 mg of the title compound (d) (yield: 90%).

後処理

  1. additionwas added to the catalyst solution
  2. filtrationfiltered
  3. concentrationconcentrated in vacuo
  4. customThe resultant was purified by Silica gel column chromatography with methanol/chloroform (1:10) solvent mixture as an eluant

出典と根拠

ORDレコード
ord-976046ffdcb14d84bd71b690132bc09f
出典データセット
uspto-grants-2010_05
特許番号
US07723376B2

反応ノート

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