Reaktion #82604

ord-6c3c3a404c6946c6be02ab29d466bc3c

Lösungsmittel

Reaktionsbedingungen

Temperatur
125°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto cool to 25° C
  2. 2
    FiltrationThe solid was collected by vacuum filtration
  3. 3
    Waschenwashed with water
  4. 4
    Sonstigedried at 40° C. under 1 mmHg for 10 h

Vorschrift

A mixture of 4,5-dibromo-1,2-phenylenediamine (1.862 g, 7.0 mmol) and oxalic acid dihydrate (1.06 g, 8.4 mmol) in 2N HCl (100 mL) was heated at 125° C. for 2 h then allowed to cool to 25° C. The solid was collected by vacuum filtration, washed with water and dried at 40° C. under 1 mmHg for 10 h affording 2.053 g (92%) of the title compound as a light brown powder. 1H NMR (DMSO-d6) 11.995 (s, 2H), 7.361 (s, 2H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05622952uspto-grants-1997_04