1,3-Cyclohexanedione, 2-chloro-2-(2-propenyl)- → 2-Cyclopenten-1-one, 2-(2-propenyl)-

HRID 372181노트

반응식

HRID 372181 반응식
Cl[C:2]1([CH2:10][CH:11]=[CH2:12])[C:7](=[O:8])[CH2:6][CH2:5][CH2:4]C1=O>C1(C)C(C)=CC=CC=1>[CH2:10]([C:2]1[C:7](=[O:8])[CH2:6][CH2:5][CH:4]=1)[CH:11]=[CH2:12]

참가 물질

3

반응물 1

HCID 122296551,3-Cyclohexanedione, 2-chloro-2-(2-propenyl)-

생성물 1

HCID 111160462-Cyclopenten-1-one, 2-(2-propenyl)-수율 50%

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

Anhydrous powdered sodium carbonate (670 g) and 1300 ml of dry (alumina) xylene were placed in a 3-l., three-necked flask equipped with a Dean-Stark trap, condenser, vibra-mixer, dropping funnel and argon inlet. The flask was flushed with argon and the contents brought to reflux. A solution of 2-chloro-2-allyl-1,3-cyclohexanedione (147 g, 0.79 mol) in 200 ml of xylene was added dropwise at such a rate that strong refluxing was maintained. After 4.5 hr, the reaction was cooled, filtered, and the sodium carbonate cake washed thoroughly with ethyl acetate. Evaporation of the solvent and careful fractionization of the residual oil gave 47.8 g (50 percent) of 2-allyl-2-cyclopenten-1-one, bp 73°-84°/4.2 mm.

후처리

  1. dry with materialAnhydrous powdered sodium carbonate (670 g) and 1300 ml of dry (alumina) xylene
  2. custom, three-necked flask equipped with a Dean-Stark trap, condenser, vibra-mixer
  3. customThe flask was flushed with argon
  4. temperatureto reflux
  5. temperaturethat strong refluxing
  6. temperaturewas maintained
  7. temperaturethe reaction was cooled
  8. filtrationfiltered
  9. washthe sodium carbonate cake washed thoroughly with ethyl acetate
  10. customEvaporation of the solvent and careful fractionization of the residual oil

출처 및 근거

ORD 기록
ord-9034c41cfb394192b1eed1d5114bd854
출처 데이터셋
uspto-grants-1978_05
특허 번호
US04089889

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