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

HRID 374343노트

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HRID 374343 반응식
[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]

참가 물질

6

반응물 3

HCID 8821Ethyl AcrylateHCID 11430Potassium CarbonateHCID 134002-Acetylcyclohexanone

생성물 1

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

시약·촉매·용매 2

HCID 66133Benzyl triethylammonium chloride촉매HCID 1140Toluene용매

반응 조건

온도
40 °C

실험 절차

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%) .

후처리

  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

출처 및 근거

ORD 기록
ord-01c5b4230fd5493da95733cce2825d6a
출처 데이터셋
uspto-grants-1992_11
특허 번호
US05166406

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