Reaktion #2275727

ord-9ab9905baa1c470ca236d29b40e48295

Reaktionsgleichung

O=c1ccccn1C1CCC2(CC1)OCCO2
1-(1,4-dioxa-spiro[4.5]dec-8-yl)-1H-pyridin-2-one
Cl
HCl
O=C([O-])O.[Na+]
sodium bicarbonate
O=C1CCC(n2ccccc2=O)CC1
title compound
O=C1CCC(n2ccccc2=O)CC1
1-(4-Oxo-cyclohexyl)-1H-pyridin-2-one

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was removed in vacuo and residue
  2. 2
    Sonstigepartitioned between ethyl acetate and water
  3. 3
    WaschenThe organic layer was washed with brine
  4. 4
    Trocknendried over anhydrous Na2SO4
  5. 5
    Filtrationfiltered
  6. 6
    Einengenconcentrated

Vorschrift

A solution of 1-(1,4-dioxa-spiro[4.5]dec-8-yl)-1H-pyridin-2-one (as prepared in the previous step, ˜300 mg, 1.28 mmol)) in acetone (10 mL) was treated with 1N HCl (2 mL) at room temperature for 4 hours. The reaction was worked up with saturated sodium bicarbonate to adjust the pH to neutral. The solvent was removed in vacuo and residue partitioned between ethyl acetate and water. The organic layer was washed with brine, dried over anhydrous Na2SO4, filtered, concentrated to afford the title compound as white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08324186B2uspto-grants-2012_12