反应详情

13.9 g (0.1 mol) 4,6-diamino-5-nitrosopyrimidine was suspended in 50 ml formamide, 6.8 g (0.1 mol) sodium formate, 27.0 g (0.5 mol) 85% formic acid and 0.5 g palladium catalyst were added according to example 1 and the mixture was heated for 4 hours to 110° C. The decolorized suspension was subsequently heated for 3 hours to 180° C. and then cooled. In order to improve the processing, 50 ml water was added and the solid was filtered. The filter cake was dissolved in 160 ml 5% sodium hydroxide solution and the insoluble Pd catalyst was separated. The clear filtrate was adjusted with sulphuric acid to a pH value of 8.5 after a 30 minute treatment at 50° C. with 3 g active carbon. In this process a colorless precipitate separated out from adenine which was suction filtered, washed twice with 30 ml water and dried in a vacuum at 80° C. 12.2 g adenine (0.090 mol, 90% of theory) was obtained in this way as a white powder.

1. temperaturethe mixture was heated for 4 hours to 110° C
2. temperatureThe decolorized suspension was subsequently heated for 3 hours to 180° C.
3. temperaturecooled
4. additionwas added
5. filtrationthe solid was filtered
6. dissolutionThe filter cake was dissolved in 160 ml 5% sodium hydroxide solution
7. customthe insoluble Pd catalyst was separated
8. customat 50° C.
9. customIn this process a colorless precipitate separated out from adenine which
10. filtrationfiltered
11. washwashed twice with 30 ml water
12. customdried in a vacuum at 80° C