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

HRID 1688728ノート

反応式

HRID 1688728 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-31ed946d7dbc47e3b3b0068e81af2f92
出典データセット
uspto-grants-2012_04
特許番号
US08148383B2

反応ノート

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