Reacción #10534

ord-addae1f9dc0349babc93745e3317e149

Condiciones de reacción

Temperatura
120°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaThe mixture was cooled to room temperature
  2. 2
    FiltraciónThe resultant solid was filtered
  3. 3
    Lavadowashed several times with water
  4. 4
    workup.DISSOLUTIONThe solid was then dissolved in dichloromethane
  5. 5
    Lavadothe solution washed with water
  6. 6
    Secadodried with anhydrous magnesium sulphate
  7. 7
    Filtraciónfiltered
  8. 8
    Otrothe solvent removed under reduced pressure
  9. 9
    OtroThe residue was azeotroped with diethyl ether (twice)

Procedimiento

A solution of N-(2,2-diphenylethyl)-2-(methylsulfonyl)-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine (Preparation 4) (20.1 g, 42.1 mmol) in dry N,N-dimethylformamide (100 ml) was treated with potassium cyanide (5.5 g, 84.6 mmol) and the mixture heated at 120° C. for 24 hours under a nitrogen atmosphere. The mixture was cooled to room temperature, poured into water (1000 ml) and stirring continued for a further 1 hour. The resultant solid was filtered and washed several times with water. The solid was then dissolved in dichloromethane and the solution washed with water, dried with anhydrous magnesium sulphate, filtered and the solvent removed under reduced pressure. The residue was azeotroped with diethyl ether (twice) to afford the title compound as an oil (17 g).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07094769B2uspto-grants-2006_08