Methanol → Methyl 3-(p-tolyl)propanoate

HRID 2261383

反応式

HRID 2261383 の反応式
[CH3:1][O:2][C:3](=[O:13])[CH:4]=[CH:5][C:6]1[CH:11]=[CH:10][C:9]([CH3:12])=[CH:8][CH:7]=1.CO.[H][H]>[Pd]>[CH3:1][O:2][C:3](=[O:13])[CH2:4][CH2:5][C:6]1[CH:7]=[CH:8][C:9]([CH3:12])=[CH:10][CH:11]=1

参加物

5

反応物 3

HCID 887MethanolHCID 589472Methyl 3-(4-methylphenyl)-2-propenoateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 9855632Methyl 3-(p-tolyl)propanoate収率 95%

試薬・触媒・溶媒 1

HCID 23938Palladium触媒

実験手順

1.39 g of 3-p-tolyl-acrylic acid methyl ester (40aa) prepared by above Step 1 was dissolved in methanol solution (7.9 mmol) under argon atmosphere. Then Pd—C was added thereto, hydrogenated under a hydrogen balloon for 1 to 2 hrs at room temperature. The reaction mixture was filtered and concentrated in vacuo. The resulting compound was purified with Silica gel column chromatography with a solvent mixture mixed with EtOAc and hexane (1:10) as an eluant to give 1.24 g of 3-p-tolyl-propionic acid methyl ester (40ab) (yield: 95%).

後処理

  1. filtrationThe reaction mixture was filtered
  2. concentrationconcentrated in vacuo
  3. customThe resulting compound was purified with Silica gel column chromatography with a solvent mixture
  4. additionmixed with EtOAc and hexane (1:10) as an eluant

出典と根拠

ORDレコード
ord-e50a6ce2bc7646af98bba2b655037b27
出典データセット
uspto-grants-2010_12
特許番号
US07846963B2

関連ノート

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