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

HRID 1277778노트

반응식

HRID 1277778 반응식
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

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 935Nickel촉매HCID 702Ethanol용매2회

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-1c927a3cef5b4357b6a58cd0ad5c5055
출처 데이터셋
uspto-grants-1981_07
특허 번호
US04278802

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