反应详情

410 mg of metallic sodium are dissolved with stirring in 100 ml of 2-ethoxy-ethanol. 1100 mg of 2,4,6-triaminonitroso-pyrimidine and 1140 mg of p-acetoxybenzyl-cyanide are added with stirring one after the other and the mixture is heated to the boiling point with stirring. The color of the mixture changes from violet to brown. After two hours' boiling under reflux, heating is discontinued and the reaction mixture is left to cool. Subsequently, 70 to 80 percent of the 2-ethoxy-ethanol are drawn off using the vacuum from a water aspirator and the residue is combined with 500 ml of water. After extraction four times with ether, the extract is adjusted to pH 5 with 2 N hydrochloric acid. The precipitate is filtered off, washed with a little ice-cold acetone and recrystallized from 10 percent acetic acid. Further purification can follow using a silica gel column. The compound mentioned in the title is obtained, which compound decomposes (with charring) at 319°-321° C.

1. temperatureis heated to the boiling point
2. stirringwith stirring
3. temperatureunder reflux
4. temperatureheating
5. waitthe reaction mixture is left
6. temperatureto cool
7. extractionAfter extraction four times with ether
8. filtrationThe precipitate is filtered off
9. washwashed with a little ice-cold acetone
10. customrecrystallized from 10 percent acetic acid
11. customFurther purification
12. customis obtained
13. customat 319°-321° C.