Reaktion #621846

ord-aa7f3269fd5945628862c4d83b8f6abc

Lösungsmittel

Reaktionsbedingungen

Temperatur
110°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeequipped with a stirrer under a nitrogen gas stream
  2. 2
    workup.STIRRINGthe reaction mixture was agitated for one hour at 140° C
  3. 3
    TemperaturThe reaction mixture was naturally cooled to room temperature
  4. 4
    Filtrationwas filtered
  5. 5
    Einengenthe filtrate was concentrated under reduced pressure
  6. 6
    workup.ADDITIONThe concentration residue was poured into water
  7. 7
    workup.STIRRINGagitated for a while
  8. 8
    Sonstigea solid that precipitated
  9. 9
    Filtrationwas collected by filtration
  10. 10
    Sonstigedried under reduced pressure

Vorschrift

Cesium fluoride (499.02 g, 3.19 mol) was added into a flask equipped with a stirrer under a nitrogen gas stream, and was agitated for one hour at 110° C. Methyl 2-chloro-3-nitrobenzoate (229.00 g, 1.06 mol) and N,N-dimethylformamide (2000 ml) were added thereto, and the reaction mixture was agitated for one hour at 140° C. The reaction mixture was naturally cooled to room temperature, and then was filtered, and the filtrate was concentrated under reduced pressure. The concentration residue was poured into water and agitated for a while, and then a solid that precipitated was collected by filtration and dried under reduced pressure. As a result, 160.03 g (yield: 76%) of the indicated compound was obtained.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08853440B2uspto-grants-2014_10