反应详情

50 g of 3,5-dichloro-pyridine are dissolved in 250 ml dimethylsulfoxide. 15 g sodium methylate are added to this solution under stirring. It is stirred under exclusion of moisture at 60°-80° C. 15 g sodium methylate are further added after each of 8 and 16 hours. After a total of 72 hours' stirring, the reaction mixture is reacted with a little water and shaked out with diethylether. The ether phase, after drying, is distilled in a vacuum, resulting in 24 g (51% of theoretical amount) of 3,5-dimethoxy-pyridine in the boiling range 90°-120° C. at 1.6·103Pa. The product is polluted with a small amount of 3-chloro-5-methoxypyridine. It can, however, be employed directly in the next stage for nitrification, since the chloro-compound is not dinitrified and therefore can easily be removed upon crystallization of the 3,5-dimethoxy-2,6-dinitro-pyridine.

1. stirringIt is stirred under exclusion of moisture at 60°-80° C
2. stirringAfter a total of 72 hours' stirring
3. dry with materialThe ether phase, after drying
4. distillationis distilled in a vacuum
5. customresulting in 24 g (51% of theoretical amount) of 3,5-dimethoxy-pyridine in the boiling range 90°-120° C. at 1.6·103Pa
6. customcan easily be removed upon crystallization of the 3,5-dimethoxy-2,6-dinitro-pyridine