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Acetone → 4-(2-Hydroxy-2-methylpropoxy)-4-methylcyclohexanone

HRID 519766
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HRID 519766 반응식
[CH3:1][C:2]([OH:17])([CH3:16])[CH2:3][O:4][C:5]1([CH3:15])[CH2:14][CH2:13][C:8]2(OCC[O:9]2)[CH2:7][CH2:6]1.Cl.CC(C)=O>O>[OH:17][C:2]([CH3:16])([CH3:1])[CH2:3][O:4][C:5]1([CH3:15])[CH2:14][CH2:13][C:8](=[O:9])[CH2:7][CH2:6]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 180AcetoneHCID 313Hydrochloric AcidHCID 670097012-Methyl-1-[(8-methyl-1,4-dioxaspiro[4.5]dec-8-yl)oxy]propan-2-ol

생성물 1

HCID 670098904-(2-Hydroxy-2-methylpropoxy)-4-methylcyclohexanone수율 71%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 2-methyl-1-[(8-methyl-1,4-dioxaspiro[4.5]dec-8-yl)oxy]propan-2-ol (1.81 g), 3N hydrochloric acid (20 mL) and acetone (20 mL) was stirred at room temperature for 18 hr. The reaction mixture was diluted with water, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel chromatography [eluent: hexane/ethyl acetate=80/20→65/35 (volume ratio)] to give the title compound as a colorless oil (1.05 g, 71%).

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후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by silica gel chromatography [eluent: hexane/ethyl acetate=80/20→65/35 (volume ratio)]

출처 및 근거

ORD 기록
ord-9494fdf69e1e404f9f5669509f308880
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09115136B2

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