Ethyl Acrylate → 2-Acetyl-2-[2-(ethoxycarbonyl)ethyl]cyclohexanone

HRID 861700

反応式

HRID 861700 の反応式
[C:1]([CH:4]1[CH2:9][CH2:8][CH2:7][CH2:6][C:5]1=[O:10])(=[O:3])[CH3:2].C(=O)([O-])[O-].[K+].[K+].[C:17]([O:21][CH2:22][CH3:23])(=[O:20])[CH:18]=[CH2:19]>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1.C1(C)C=CC=CC=1>[C:1]([C:4]1([CH2:19][CH2:18][C:17]([O:21][CH2:22][CH3:23])=[O:20])[CH2:9][CH2:8][CH2:7][CH2:6][C:5]1=[O:10])(=[O:3])[CH3:2]

参加物

6

反応物 3

HCID 8821Ethyl AcrylateHCID 11430Potassium CarbonateHCID 134002-Acetylcyclohexanone

生成物 1

HCID 190674842-Acetyl-2-[2-(ethoxycarbonyl)ethyl]cyclohexanone収率 97%

試薬・触媒・溶媒 2

HCID 66133Benzyl triethylammonium chloride触媒HCID 1140Toluene溶媒

反応条件

温度
40 °C

実験手順

To a solution of 2-acetylcyclohexanone (25 g, 0.18 mol), potassium carbonate (29.5 g, 0.21 mol) and benzyltriethylammonium chloride (0.8 g, 0.0035 mol) in toluene (70 ml) was added ethyl acrylate (29 ml, 27 g, 0.27 mol) at room temperature. The mixture was heated at 40° C. for 20 hours, filtered and partitioned between distilled water (200 ml) and toluene (200 ml). The organic layer was dried over magnesium sulphate, filtered and concentrated under reduced pressure to give the title compound as a brown oil, (41.7 g, 97%).

後処理

  1. filtrationfiltered
  2. custompartitioned
  3. distillationbetween distilled water (200 ml) and toluene (200 ml)
  4. dry with materialThe organic layer was dried over magnesium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-84e3928876e44891a380435e78496325
出典データセット
uspto-grants-1998_02
特許番号
US05714628

関連ノート

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