Reaktion #1903940

ord-bf83582fd3f34a07af32db04b838af68

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added to the mixture
  2. 2
    WaschenThe organic layer was washed with sodium chloride solution
  3. 3
    Trocknendried over magnesium sulfate
  4. 4
    FiltrationThe magnesium sulfate was filtered off
  5. 5
    Einengenthe filtrate was concentrated under reduced pressure

Vorschrift

To a solution of 4-(cis-2,6-dimethylmorpholin-4-yl)benzoic acid ethyl ester (0.55 g) in a mixed solvent of methanol (3 ml) and tetrahydrofuran (6 ml) was added hydrazine monohydrate (1.6 ml). The solution was refluxed for 20 hours, during which period additional hydrazine monohydrate (1.6 ml) was added to the mixture. After cooling to ambient temperature, the reaction mixture was added to a mixture of water and ethyl acetate. The organic layer was washed with sodium chloride solution. The organic layer was taken and dried over magnesium sulfate. The magnesium sulfate was filtered off, and the filtrate was concentrated under reduced pressure to give 4-(cis-2,6-dimethylmorpholin-4-yl)benzoic acid hydrazide (489.7 mg).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06884868B1uspto-grants-2005_04