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

HRID 1660458노트

반응식

HRID 1660458 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 were 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-6186a229d2314f96b391e1f6e7ac94d2
출처 데이터셋
uspto-grants-1981_12
특허 번호
US04308208

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