Dimethyl Ether → 4-Methoxy-4-phenylcyclohexanone

HRID 1816349노트

반응식

HRID 1816349 반응식
[CH3:1][O:2][C:3]1([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:12][CH2:11][C:6]2(OCC[O:7]2)[CH2:5][CH2:4]1.C(=O)([O-])O.[Na+].COC>O1CCCC1>[CH3:1][O:2][C:3]1([C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH2:12][CH2:11][C:6](=[O:7])[CH2:5][CH2:4]1

참가 물질

5

반응물 3

HCID 8254Dimethyl EtherHCID 516892Sodium BicarbonateHCID 224929828-Methoxy-8-phenyl-1,4-dioxaspiro[4.5]decane

생성물 1

HCID 224929924-Methoxy-4-phenylcyclohexanone수율 73.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 8-methoxy-8-phenyl-1,4-dioxaspiro[4.5]decane (5.96 g) and 3N-hydrrochloric acid (24 ml) in tetrahydrofuran was stirred at room temperature for 24 hours. The reaction mixture was added to a mixture of sodium hydrogen carbonate solution and dimethyl ether. The organic layer was washed with sodium hydrogen carbonate solution and dried over magnesium sulfate. The magnesium sulfate was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel chromatography (1:0-150:1 dichloromethane-methanol elution) to give 4-methoxy-4-phenylcyclohexanone (3.6 g).

후처리

  1. washThe organic layer was washed with sodium hydrogen carbonate solution
  2. dry with materialdried over magnesium sulfate
  3. filtrationThe magnesium sulfate was filtered off
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue was purified by silica gel chromatography (1:0-150:1 dichloromethane-methanol elution)

출처 및 근거

ORD 기록
ord-7ee3d31164234e8698c29714a813150d
출처 데이터셋
uspto-grants-2005_04
특허 번호
US06884774B2

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