Phosphorus oxychloride → 3,4-Dihydro-4,4-dimethyl-2H-pyran-2-one

HRID 67040노트

반응식

HRID 67040 반응식
[CH3:1][C:2]([CH3:12])([CH2:9][CH:10]=O)[CH2:3][C:4]([O:6]CC)=[O:5].P(Cl)(Cl)(Cl)=O>C1(C)C=CC=CC=1.CCOCC>[CH3:12][C:2]1([CH3:1])[CH:9]=[CH:10][O:6][C:4](=[O:5])[CH2:3]1

참가 물질

5

반응물 2

HCID 24813Phosphorus oxychlorideHCID 13050815Ethyl 4-formyl-3,3-dimethylbutanoate

생성물 1

HCID 30186853,4-Dihydro-4,4-dimethyl-2H-pyran-2-one수율 40.1%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 3283Diethyl Ether용매

실험 절차

A solution of 11.16 g (0.065 mole) of ethyl 3,3-dimethyl-5-oxopentanoate and 11.2 g (0.073 mole) of phosphoryl chloride in 90 ml of toluene was heated under reflux for 14 hours. The mixture was diluted with ether, washed with an aqueous solution of sodium bicarbonate, dried over anhydrous magnesium sulfate, filtered, and the filtrate concentrated to give, after distillation, 3.29 g (40% yield) of 3,4-dihydro-4,4-dimethyl-2H-pyran-2-one, bp 105°-110° C./2670 Pa (20 mm Hg).

후처리

  1. temperatureunder reflux for 14 hours
  2. washwashed with an aqueous solution of sodium bicarbonate
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationthe filtrate concentrated
  6. customto give

출처 및 근거

ORD 기록
ord-77fb5c9d2f004ba8a6cb5829930cf35a
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04344884

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