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

HRID 1412475ノート

反応式

HRID 1412475 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 670089144-(2-Hydroxy-2-methylpropoxy)cyclohexanone収率 73%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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%).

後処理

  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)]

出典と根拠

ORDレコード
ord-d5be94f3b1b6432395e142c73d9d60af
出典データセット
uspto-grants-2014_12
特許番号
US08921379B2

反応ノート

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