Hydrochloric Acid → 4-Hydroxy-4-methylcyclohexanone

HRID 509282

Reaktionsgleichung

Reaktionsgleichung von HRID 509282
[CH3:1][C:2]1([OH:12])[CH2:11][CH2:10][C:5]2(OCC[O:6]2)[CH2:4][CH2:3]1.Cl>C1COCC1>[OH:12][C:2]1([CH3:1])[CH2:11][CH2:10][C:5](=[O:6])[CH2:4][CH2:3]1

Komponenten

4

Versuchsvorschrift

8-Methyl-1,4-dioxaspiro[4.5]decane-8-ol (650 mg, 3.77 mmol) was dissolved in THF (10 ml), followed by addition of 1N aqueous HCl solution (5 ml), and then the resulting mixture was stirred at room temperature for 6 hours. The resulting reaction liquid was concentrated under reduced pressure, and then extracted with 10% MeOH/MC (20 ml×5). The organic layer was dried over anhydrous sodium sulfate, followed by filtration and concentration, and then the residue thus obtained was subjected to MPLC (50% EtOAc/Hexanes), to obtain 443 mg of yellow oil (92%).

Aufarbeitung

  1. customThe resulting reaction liquid
  2. concentrationwas concentrated under reduced pressure
  3. extractionextracted with 10% MeOH/MC (20 ml×5)
  4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  5. filtrationfollowed by filtration and concentration
  6. customthe residue thus obtained

Quellen und Nachweise

ORD-Eintrag
ord-4c8d104f2237465ead45294b8349f757
Quelldatensatz
uspto-grants-2015_08
Patentnummer
US09096571B2

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