Methyl alpha-methylthio-alpha-(m-(alpha,alpha-dimethoxybenzyl)phenyl)propionate → Methyl alpha-[m-(alpha,alpha-dimethoxybenzyl)phenyl]propionate

HRID 1277778ノート

反応式

HRID 1277778 の反応式
CS[C:3]([C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([O:24][CH3:25])([O:22][CH3:23])[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:10]=1)([CH3:8])[C:4]([O:6][CH3:7])=[O:5]>C(O)C.[Ni]>[CH3:23][O:22][C:15]([C:11]1[CH:10]=[C:9]([CH:3]([CH3:8])[C:4]([O:6][CH3:7])=[O:5])[CH:14]=[CH:13][CH:12]=1)([O:24][CH3:25])[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1

参加物

4

反応物 1

HCID 12819452Methyl alpha-methylthio-alpha-(m-(alpha,alpha-dimethoxybenzyl)phenyl)propionate

生成物 1

HCID 12819453Methyl alpha-[m-(alpha,alpha-dimethoxybenzyl)phenyl]propionate収率 86.4%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 702Ethanol溶媒2 回

実験手順

Methyl α-methylthio-α-[m-(α,α-dimethoxybenzyl)phenyl]-propionate (211 mg) was dissolved in 1 ml of ethanol, and 5 ml of an ethanol suspension of 2 cc of Raney nickel (W-II) was added. The mixture was stirred at room temperature for 1 hour. The insoluble matter was separated by filtration, and washed with 40 ml of ethanol. The filtrate and the washing are combined and concentrated under reduced pressure, and 30 ml of methylene chloride was added to the residue. The insoluble matter was separated by filtration, and the solvent was evaporated off under reduced pressure to afford 159 mg of methyl α-[m-(α,α-dimethoxybenzyl)phenyl]propionate as an oil in a yield of 86%.

後処理

  1. additionwas added
  2. customThe insoluble matter was separated by filtration
  3. washwashed with 40 ml of ethanol
  4. concentrationconcentrated under reduced pressure, and 30 ml of methylene chloride
  5. additionwas added to the residue
  6. customThe insoluble matter was separated by filtration
  7. customthe solvent was evaporated off under reduced pressure

出典と根拠

ORDレコード
ord-1c927a3cef5b4357b6a58cd0ad5c5055
出典データセット
uspto-grants-1981_07
特許番号
US04278802

反応ノート

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