| 5-amino-6-nitro-[1,2,5] oxadiazolo[3,4-b]pyridine-l-oxide was prepared from 2,6-dichl-oropyridine by nitration, ammoniation, nitration, azido reaction, thermolysis. The important factors of each reaction were studied based on the experiment. The optimal process condictions of each unit reaction were optimimized.Optimal conditions of nitration were obtained as follows:2,6-dichloropyridine 5.0g, concentrated sulfuric acid 14mL,mixed acid 6mL, reacting at 110℃for 5h, the yield was79.36%.Optimal conditions of ammoniation were obtained as follows:2,6-dichloro-3-nit-ropyridine19.3g, anhydrous ethanol 100mL, reacting at room temperature, the yield was 89.97%.Optimal conditions of nitration were obtained as follows:2-amino-6-chloro-3-nitrop-yridine 3.5g, concentrated sulfuric acid 20mL, potassium nitrate 2.5g, reacting at 40℃for 6h, the yield was 78.30%. Optimal conditions of azido reaction were obtained as follows: 2-amino-6-chloro-3,5- dinitropyridine 3.7g,acetone 50mL,sodium azide 1.7g,water 15mL, reacting at 20℃for 30min, the yield was 88.61%.Optimal conditions of thermolysis were obtained as follows:4,6-dinitro-7- aminotetrazolo[1,5-a]pyridine 1.Og, 100mL toluene as solvent, reacting at 110℃for 1.Oh, the yield was 95.14%. Total yield was 47.13%.The product was characterized by IR, MS,and 1HNMR. |
