反应详情

温度

120 °C

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).

1. temperatureThe mixture was cooled to room temperature
2. filtrationThe resultant solid was filtered
3. washwashed several times with water
4. dissolutionThe solid was then dissolved in dichloromethane
5. washthe solution washed with water
6. dry with materialdried with anhydrous magnesium sulphate
7. filtrationfiltered
8. customthe solvent removed under reduced pressure
9. customThe residue was azeotroped with diethyl ether (twice)