Reaktion #359645

ord-fa91249b3985490b8206df69023cea64

Lösungsmittel

Reaktionsbedingungen

Temperatur
120°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solid formed
  2. 2
    Temperaturupon cooling
  3. 3
    Filtrationwas collected by filtration
  4. 4
    Waschenwashed with toluene
  5. 5
    Sonstigesonicated in hot MeOH
  6. 6
    FiltrationAfter filtration the solid
  7. 7
    Sonstigewas dried further

Vorschrift

A mixture of 6-bromo-8-cyclopentyl-2-methanesulfinyl-5-methyl-8H-pyrido[2,3-d]pyrimidin-7-one (370 mg, 1.0 mmol) and 2,6-diaminopyridine (163 mg, 1.5 mmol) in toluene (5 mL) was heated at 120° C. overnight. The solid formed upon cooling was collected by filtration, washed with toluene and sonicated in hot MeOH. After filtration the solid was dried further to give the desired product 2-(6-amino-pyridin-2-ylamino)-6-bromo-8-cyclopentyl-5-methyl-8H-pyrido[2,3-d]pyrimidin-7-one (39 mg, 9.3%). mp: >274.6˜276° C. Calc'd for C18H19BrN6O.0.2H2O: C, 51.61; H, 4.67; N,20.06. Found: C, 51.42; H, 4.44; N, 19.87.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07456168B2uspto-grants-2008_11