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

HRID 67040ノート

反応式

HRID 67040 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 3283Diethyl Ether溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-77fb5c9d2f004ba8a6cb5829930cf35a
出典データセット
uspto-grants-1982_08
特許番号
US04344884

反応ノート

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