反应详情

3-(3-nitrophenyl)pyridine (50 g, 0.25 mol) was added portion-wise with stirring to dimethyl sulfate (125 ml). The mixture was stirred at ambient temperature for 24 hours, during which time additional dimethyl sulfate was added (2×50 ml). At the end of the reaction diethyl ether (400 ml) was added, and the mixture was stirred in the cold for 2 hours. The precipitate was filtered off and washed several times with diethyl ether. Finally, the precipitate was stirred in pyridine (100 ml) at 45° C. for 30 min. THF (250 ml) was added. Stirring was continued for additionally 30 min whereafter the product was filtered off, washed with diethyl ether and dried to yield 1-methyl-3-(3-nitrophenyl)pyridinium methyl sulfate (66.6 g, 82%).

1. additionwas added (2×50 ml)
2. additionwas added
3. filtrationThe precipitate was filtered off
4. washwashed several times with diethyl ether
5. stirringFinally, the precipitate was stirred in pyridine (100 ml) at 45° C. for 30 min
6. additionTHF (250 ml) was added
7. stirringStirring
8. waitwas continued for additionally 30 min whereafter the product
9. filtrationwas filtered off
10. washwashed with diethyl ether
11. customdried