Reaktion #157309

ord-19e6337ddada4661bb84eebb88a950a1

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto reflux overnight
  2. 2
    Einengenthe reaction mixture was concentrated under reduced pressure
  3. 3
    Filtrationcollected by filtration
  4. 4
    Waschenwashed with water (2×)
  5. 5
    Sonstigeair-dried
  6. 6
    SonstigeFurther drying in a 35° C. vacuum oven

Vorschrift

3-Hydroxy-2-aminopyridine (2.00 g, 18.2 mmol) and potassium hydroxide (1.22 g, 21.8 mmol) were dissolved in carbon disulfide (15 mL) and EtOH (25 mL), and the reaction mixture was heated to reflux overnight. Upon cooling to rt, the reaction mixture was concentrated under reduced pressure. The resulting solid was suspended in 1 M aqueous HCl, collected by filtration, washed with water (2×) and air-dried. Further drying in a 35° C. vacuum oven gave 2.52 g (91%) of the title compound as a tan solid. LC-MS: RT=4.82 min., [M+H]+=153.1

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08822472B2uspto-grants-2014_09