4-Benzoyloxy-1-hydroxy-1-hexene-3,5-dione → 3-(Benzoyloxy)-2-methyl-4H-pyran-4-one

HRID 1461541노트

반응식

HRID 1461541 반응식
[C:1]([O:9][CH:10]([C:16](=[O:18])[CH3:17])[C:11](=[O:15])[CH:12]=[CH:13]O)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>C(O)(=O)C>[C:1]([O:9][C:10]1[C:11](=[O:15])[CH:12]=[CH:13][O:18][C:16]=1[CH3:17])(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

3

반응물 1

HCID 679144844-Benzoyloxy-1-hydroxy-1-hexene-3,5-dione

생성물 1

HCID 802553-(Benzoyloxy)-2-methyl-4H-pyran-4-one수율 81.2%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

4-Benzoyloxy-1-hydroxy-1-hexene-3,5-dione (54.20 g, 218 mmol) is refluxed for 2 hours in 400 ml of acetic acid, the reaction mixture is concentrated at 40° C. on a rotary evaporator, the residue is dissolved in 500 ml of dichloromethane and washed twice with 300 ml of saturated sodium bicarbonate solution. The organic phase is dried over magnesium sulphate, concentrated on a rotary evaporator and gives 40.75 g (81.2%) of 3-benzoyloxy-2-methyl-4-pyrone, content 73%, m.p.: 106°-110° C.

후처리

  1. concentrationthe reaction mixture is concentrated at 40° C. on a rotary evaporator
  2. dissolutionthe residue is dissolved in 500 ml of dichloromethane
  3. washwashed twice with 300 ml of saturated sodium bicarbonate solution
  4. dry with materialThe organic phase is dried over magnesium sulphate
  5. concentrationconcentrated on a rotary evaporator

출처 및 근거

ORD 기록
ord-c4ade3ba5ef4402c9430bb0ff261f7d1
출처 데이터셋
uspto-grants-1991_12
특허 번호
US05075461

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