反应详情

温度

70 °C

10 g (0.25 mol) of sodium hydroxide dissolved in 100 ml of water were added to a suspension of 52 g (0.25 mol) of 3-butylxanthine in 300 ml of methanol and the reaction mixture was stirred at 70° C. for one hour, then treated dropwise at the same temperature with 42.8 g (0.25 mol) of benzyl bromide and kept between 70° and 80° C. for 5 hours. 1.0 g (0.025 mol) of sodium hydroxide and 4.28 g (0.025 mol) of benzyl bromide were then added. After a further 2 hours, the mixture was cooled, diluted with 1500 ml of water and filtered cold on a suction filter, the product was washed with water on the suction filter and dissolved in 1000 ml of 1 N sodium hydroxide solution, and the solution was filtered and slowly brought to pH 3 with stirring using concentrated hydrochloric acid. The crystallizate was filtered off from the solution, washed with water until chloride-free and dried under reduced pressure.

1. waitkept between 70° and 80° C. for 5 hours
2. waitAfter a further 2 hours
3. temperaturethe mixture was cooled
4. filtrationfiltered cold on a suction
5. filtrationfilter
6. washthe product was washed with water on the suction
7. filtrationfilter
8. dissolutiondissolved in 1000 ml of 1 N sodium hydroxide solution
9. filtrationthe solution was filtered
10. stirringwith stirring
11. filtrationThe crystallizate was filtered off from the solution
12. washwashed with water until chloride-free
13. customdried under reduced pressure