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

HRID 1688728노트

반응식

HRID 1688728 반응식
O1[C:5]2([CH2:10][CH2:9][CH:8]([O:11][CH2:12][C:13]([CH3:16])([OH:15])[CH3:14])[CH2:7][CH2:6]2)[O:4]CC1.Cl.CC(C)=O>O>[OH:15][C:13]([CH3:16])([CH3:14])[CH2:12][O:11][CH:8]1[CH2:9][CH2:10][C:5](=[O:4])[CH2:6][CH2:7]1

참가 물질

5

반응물 3

HCID 180AcetoneHCID 313Hydrochloric AcidHCID 670091781-(1,4-Dioxaspiro[4.5]dec-8-yloxy)-2-methylpropan-2-ol

생성물 1

HCID 670089144-(2-Hydroxy-2-methylpropoxy)cyclohexanone수율 73%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 1-(1,4-dioxaspiro[4.5]dec-8-yloxy)-2-methylpropan-2-ol (5.53 g), 3N hydrochloric acid (30 mL) and acetone (30 mL) was stirred at room temperature for 16 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→60/40 (volume ratio)] to give the title compound as a colorless oil (3.25 g, 73%).

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→60/40 (volume ratio)]

출처 및 근거

ORD 기록
ord-31ed946d7dbc47e3b3b0068e81af2f92
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08148383B2

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