Reaktion #88405

ord-1d414470be0b476fab1ac89e737035b4

Lösungsmittel

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGthe obtained mixture was then stirred for 6 hours at the same temperature
  2. 2
    EinengenThereafter, the reaction solution was concentrated under reduced pressure, and ethyl acetate (10 ml)
  3. 3
    workup.ADDITIONwas then added to the obtained residue
  4. 4
    FiltrationThe precipitated solid was collected by filtration, and it
  5. 5
    Waschenwas washed with ethyl acetate (15 ml) and heptane (6 ml)
  6. 6
    Sonstigewas then dried

Vorschrift

2-Bromo-1-(2,5-difluorophenyl)ethanone (1.5 g) was added to an ethanol (8.2 ml) solution of methyl 2-aminoisonicotinate (1.0 g), and the obtained mixture was then stirred in a nitrogen atmosphere at 60° C. for 18 hours. Thereafter, 2-bromo-1-(2,5-difluorophenyl)ethanone (0.77 g) was added to the reaction solution, and the obtained mixture was then stirred for 6 hours at the same temperature as described above. Thereafter, the reaction solution was concentrated under reduced pressure, and ethyl acetate (10 ml) was then added to the obtained residue. The precipitated solid was collected by filtration, and it was washed with ethyl acetate (15 ml) and heptane (6 ml) and was then dried, so as to obtain the title compound (2.5 g) in the form of a pink solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09440970B2uspto-grants-2016_09