Reaktion #65774

ord-2bf35121bb444064bd6214b7aec6662a

Lösungsmittel

Reaktionsbedingungen

Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe resulting precipitate was collected by filtration
  2. 2
    Waschenwashed with water
  3. 3
    Sonstigefollowed by reprecipitation from DMSO-H2O

Vorschrift

To 0.35 g of 3-amino-6-chloro-4,5-diethoxycarbonyl-2-(3-aminophenyl)pyridine was added 7.5 ml of hydrazine monohydrate, and the mixture was stirred at 90° C. for 30 minutes. The reaction mixture was poured into ice water (100 ml), and the mixture was adjusted to pH 6 by adding acetic acid. The resulting precipitate was collected by filtration and washed with water, followed by reprecipitation from DMSO-H2O, to give 0.23 g of the title compound as orange powder.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05420275uspto-grants-1995_05