Ethyl Acetate → HCID 54452584, 화합물

HRID 377307

반응식

HRID 377307 반응식
C(C(CC)(P(O)(O)=O)C(O)=O)C.[H-].[Na+].[CH3:15][O:16][C:17]1[CH:18]=[C:19]([CH:23]2[CH2:27][CH2:26][CH2:25][C:24]2=O)[CH:20]=[CH:21][CH:22]=1.[C:29]([O:32][CH2:33][CH3:34])(=[O:31])[CH3:30]>COCCOC.O>[CH3:15][O:16][C:17]1[CH:18]=[C:19]([CH:23]2[CH2:27][CH2:26][CH2:25][C:24]2=[CH:30][C:29]([O:32][CH2:33][CH3:34])=[O:31])[CH:20]=[CH:21][CH:22]=1

참가 물질

7

반응물 4

HCID 8857Ethyl AcetateHCID 24758Sodium hydrideHCID 123629382-(3-Methoxyphenyl)cyclopentan-1-oneHCID 17786294Diethyl phosphonoacetic acid

생성물 1

HCID 54452584HCID 54452584, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 80711,2-Dimethoxyethane용매2회

실험 절차

To a solution of diethyl phosphono acetic acid (8.0 ml) in 1,2-dimethoxyethane (80 ml) was added sodium hydride (60% in oil, 1.4 g) at 0° C. under N2. After being stirred for 1 hour at ambient temperature, to the solution was added a solution of 2-(3-methoxyphenyl)cyclopentanone (4.5 g) in 1,2-dimethoxyethane (20 ml). After being stirred for 12 hours, the reaction mixture was poured into a mixture of ethyl acetate and water. The organic layer was washed with saturated sodium bicarbonate aqueous solution and brine. The dried solvent was concentrated and the obtained residue was purified by column chromatography on silica gel to give ethyl [2-(3-methoxyphenyl)cyclopentylidene]acetate (5.0 g).

후처리

  1. stirringAfter being stirred for 12 hours
  2. washThe organic layer was washed with saturated sodium bicarbonate aqueous solution and brine
  3. concentrationThe dried solvent was concentrated
  4. customthe obtained residue was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-ad95da0c036d498085df69c8c0bc077e
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06025375

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