Ethyl Acetate → HCID 54452584、化合物

HRID 377307

反応式

HRID 377307 の反応式
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

参加物

7

反応物 4

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

生成物 1

HCID 54452584HCID 54452584、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 80711,2-Dimethoxyethane溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-ad95da0c036d498085df69c8c0bc077e
出典データセット
uspto-grants-2000_02
特許番号
US06025375

関連ノート

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