Reaktion #160675

ord-92579535052540ec95de14424f4d8df3

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter removal of the solvent
  2. 2
    Sonstigethe residue is chromatographed on silica gel using
  3. 3
    workup.ADDITIONa mixture of petroleum ether/ethyl acetate in the ratio 2/1

Vorschrift

10.18 g of (1RS,3RS,4RS)-3-(3,4-dimethoxyphenyl)-4-nitrocydohexanol (compound D2) are dissolved in 100 ml of acetic anhydride and the solution is heated to 100° C. for 1-2 h. After removal of the solvent, the residue is chromatographed on silica gel using a mixture of petroleum ether/ethyl acetate in the ratio 2/1. Concentration of the corresponding eluate fractions furnish 10.37 g (89% of theory) of the title compound as an oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08829189B2uspto-grants-2014_09