Reaktion #92675

ord-a3c237c8dcc249478fb8b1f6f5f2c6ba

Reaktionsbedingungen

Temperatur
78°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeAfter leaving
  2. 2
    Temperaturto be cooled at room temperature, to the reaction mixture
  3. 3
    Sonstigea layer separation operation
  4. 4
    WaschenThe organic layer was washed with water and saturated brine
  5. 5
    Trocknendried over anhydrous magnesium sulfate
  6. 6
    Sonstigethe solvent was evaporated under reduced pressure

Vorschrift

A suspension of 1 g of 5-methyl-2-nitropyridin-3-ol, 1.35 ml of (bromomethyl)cyclohexane, and 1.79 g of potassium carbonate in 10 ml of DMF was stirred at 78° C. for 12 hours. After leaving to be cooled at room temperature, to the reaction mixture were added water and hexane/ethyl acetate to carry out a layer separation operation. The organic layer was washed with water and saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure to obtain 1.8 g of 3-(cyclohexylmethoxy)-5-methyl-2-nitropyridine.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09447090B2uspto-grants-2016_09