Reaktion #1519103

ord-d9301c198d864dcfa44e24684afd95e0

Reaktionsgleichung

CCOC(=O)CC(=O)c1cc(Cl)ccn1
3-(4-chloropyrid-2-yl)-3-oxopropionic acid ethyl ester
Cl.N=C(N)c1ccccn1
2-amidinopyridine hydrochloride
[Na+].[OH-]
sodium hydroxide
Oc1cc(-c2cc(Cl)ccn2)nc(-c2ccccn2)n1
6-(4-chloropyrid-2-yl)-2-pyrid-2-yl-pyrimidin-4-ol

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturrefluxing
  2. 2
    TemperaturThe mixture is cooled
  3. 3
    Einengenconcentrated to a fifth of its original volume
  4. 4
    FiltrationThe crude product is filtered off
  5. 5
    Sonstigerecrystallised from methanol

Vorschrift

13.15 g (58 mmol) of 3-(4-chloropyrid-2-yl)-3-oxopropionic acid ethyl ester are dissolved in 400 ml of ethanol, and 9.10 g (58 mmol) of 2-amidinopyridine hydrochloride are added. After the addition of 14.44 ml of 4N sodium hydroxide solution, refluxing is carried out for 7 hours. The mixture is cooled and concentrated to a fifth of its original volume. The crude product is filtered off and recrystallised from methanol, yielding 6-(4-chloropyrid-2-yl)-2-pyrid-2-yl-pyrimidin-4-ol in the form of beige needles.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07612010B2uspto-grants-2009_11