Reacción #10534
ord-addae1f9dc0349babc93745e3317e149
Ecuación de reacción
Reactantes
Reactivos
Disolventes
Condiciones de reacción
Tratamiento posterior
- 1TemperaturaThe mixture was cooled to room temperature
- 2FiltraciónThe resultant solid was filtered
- 3Lavadowashed several times with water
- 4workup.DISSOLUTIONThe solid was then dissolved in dichloromethane
- 5Lavadothe solution washed with water
- 6Secadodried with anhydrous magnesium sulphate
- 7Filtraciónfiltered
- 8Otrothe solvent removed under reduced pressure
- 9OtroThe 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).