反应详情

To a suspension of 6-[(2,2-diphenylethyl)amino]-9-(tetrahydro-2H-pyran-2-yl) 9H-purine-2-carboxylic acid (249 g, 0.561 moles) (Preparation 21) in anhydrous tetrahydrofuran (2500 ml) was added N,N′-carbonyldiimidazole (109 g, 0.672 moles) in two portions over 10 minutes. The resulting mixture was stirred at ambient temperature under an atmosphere of nitrogen whereupon the solid gradually dissolved to give a cloudy pale orange solution. After stirring for 2.5 h, the reaction mixture was cooled in an ice-bath, and a solution of 2-(1-piperidinyl)ethylamine (86.4 g, 0.674 moles) in anhydrous tetrahydrofuran (100 ml) was added over a period of 55 minutes during which time a clear orange solution formed. The reaction mixture was stirred at room temperature for a further 17.5 hours. Deionised water (10 ml) was then added and the reaction mixture was then distilled at atmospheric pressure until approximately 2400 ml of distillate had collected. To the resultant amber oil was added isopropanol (2000 ml) and distillation at atmospheric pressure was continued until approximately 50 ml of distillate had collected. The resultant dark orange solution was allowed to cool to ambient temperature and further isopropanol (600 ml) was added to give a solution of the title compound in isopropanol that may be used directly without further purification.

1. dissolutiongradually dissolved
2. customto give a cloudy pale orange solution
3. stirringAfter stirring for 2.5 h
4. temperaturethe reaction mixture was cooled in an ice-bath
5. customformed
6. stirringThe reaction mixture was stirred at room temperature for a further 17.5 hours
7. distillationthe reaction mixture was then distilled at atmospheric pressure until approximately 2400 ml of distillate
8. customhad collected
9. additionTo the resultant amber oil was added
10. distillationisopropanol (2000 ml) and distillation at atmospheric pressure
11. customhad collected
12. temperatureto cool to ambient temperature
13. additionfurther isopropanol (600 ml) was added