Acetic Acid → 1-Oxo-1-(2-oxocyclopentyl)propan-2-yl acetate

HRID 240897

반응식

HRID 240897 반응식
[C:1]([O:4][CH:5]([CH3:18])[C:6](=[O:17])[C:7]1[CH2:11][CH2:10][CH2:9][C:8]=1N1CCCC1)(=[O:3])[CH3:2].C(O)(=[O:21])C>O1CCCC1.O.ClCCl>[C:1]([O:4][CH:5]([CH3:18])[C:6](=[O:17])[CH:7]1[CH2:11][CH2:10][CH2:9][C:8]1=[O:21])(=[O:3])[CH3:2]

참가 물질

6

반응물 2

HCID 176Acetic AcidHCID 710141241-Oxo-1-(2-(pyrrolidin-1-yl)cyclopent-1-enyl)propan-2-yl acetate

생성물 1

HCID 141483511-Oxo-1-(2-oxocyclopentyl)propan-2-yl acetate

시약·촉매·용매 3

HCID 962Water용매2회HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

실험 절차

Stir a mixture of 1-oxo-1-(2-(pyrrolidin-1-yl)cyclopent-1-enyl)propan-2-yl acetate (952.0 g), acetic acid (1500 mL) and water (1500 mL) in tetrahydrofuran (3000 mL) at room temperature for 2 days. Dilute the mixture with water (1200 mL) and dichloromethane (1200 mL). The organic layer is washed with brine, dried over anhydrous Na2SO4 and concentrated under vacuum. Purify the residue by silica gel chromatograph (eluting with 3% to 10% ethyl acetate in petroleum ether) to give 1-oxo-1-(2-oxocyclopentyl)propan-2-yl acetate as oil (573.4 g, 2.89 mol, 72.6% for 2 steps).

후처리

  1. washThe organic layer is washed with brine
  2. dry with materialdried over anhydrous Na2SO4
  3. concentrationconcentrated under vacuum
  4. customPurify the residue
  5. washby silica gel chromatograph (eluting with 3% to 10% ethyl acetate in petroleum ether)

출처 및 근거

ORD 기록
ord-e1956981e08d4204b90cd849cbdf31eb
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08648081B2

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