Reacción #607730

ord-62e171210a264b969368e921b7d8705d

Disolventes

Condiciones de reacción

Temperatura
70°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    ConcentraciónThe solvent was partially concentrated in vacuo
  2. 2
    Otroto remove the methanol
  3. 3
    Extracciónextracted with ethyl acetate (3×20 ml)
  4. 4
    OtroThe combined organic layers were dried
  5. 5
    Concentraciónconcentrated

Procedimiento

Methyl [(2R,6S)-2,6-dimethyl-4-morpholinyl]acetate (5.05 g, 27.0 mmol, see Journal of Fluorine Chemistry (1998) 193-201 for literature preparation) was dissolved in methanol (20 ml) and hydrazine hydrate (2.013 ml, 27.0 mmol) added. The reaction mixture was heated to 70° C. for 18 h. The solvent was partially concentrated in vacuo to remove the methanol and extracted with ethyl acetate (3×20 ml). The combined organic layers were dried and concentrated to afford the title compound as a yellow solid (3.35 g).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US09326987B2uspto-grants-2016_05