Reaktion #709269

ord-75cff03e37a54438ac6cedfbf90b27af

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturAfter cooling
  2. 2
    Filtrationthe salts are filtered off with suction
  3. 3
    Sonstigethe solution is evaporated
  4. 4
    Waschenthe mixture is washed with water
  5. 5
    SonstigeThe organic phase is dried
  6. 6
    Einengenconcentrated
  7. 7
    Sonstigethe residue is chromatographed on silica gel with chloroform with 1% of methanol
  8. 8
    SonstigeIntensely yellow crystals are obtained from ethanol

Vorschrift

2 g (4.7 mmol) of 2-methyl-8a-morpholino-3-nitro-4-(2-trifluoromethylphenyl)-4a,5,6,7,8,8a-hexahydro-4H-chromene are heated at the reflux temperature in 15 ml of ethanol with 2 g of methylammonium chloride for 6 hours. After cooling, the salts are filtered off with suction, the solution is evaporated, the residue is taken up in chloroform and the mixture is washed with water. The organic phase is dried and concentrated and the residue is chromatographed on silica gel with chloroform with 1% of methanol. Intensely yellow crystals are obtained from ethanol.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04769375uspto-grants-1988_09