反应详情

2 g (16.4 mmol) of 5-amino-2-ethylpyridine (for the preparation see G. H. Cooper and R. L. Rickard, J. Chem. Soc. C, 3257-60 (1971) are dissolved in 17.7 ml of concentrated HCl, and 2.2 ml (21.4 mol) of 30% strength H2O2 solution are then carefully added. An exothermic reaction starts. The temperature is kept at about 50° C. by cooling with an ice-bath, and when the reaction has subsided the mixture is subsequently stirred at this temperature for a further 15 minutes. For working up, the mixture is poured onto 200 ml of water, the pH is brought to 10 with 40% strength sodium hydroxidde solution and the mixture is extracted twice with 100 ml of methylene chloride each time. After drying with Na2SO4, the mixture is evaporated and the residue is stirred with petroleum ether and filtered off with suction.

1. customAn exothermic reaction
2. customis kept at about 50° C.
3. temperatureby cooling with an ice-bath
4. extractionthe mixture is extracted twice with 100 ml of methylene chloride each time
5. dry with materialAfter drying with Na2SO4
6. customthe mixture is evaporated
7. stirringthe residue is stirred with petroleum ether
8. filtrationfiltered off with suction