反应详情

30 ml of 100% nitric acid is added to 150 ml of 98% sulphuric acid with stirring and cooling. To this solution is added dropwise 3.2 g (26 mmol) of 3-methyl-4-methoxy pyridine. The mixture is stirred at 80° C. for 2.5 hours, cooled down and added cautiously to a mixture of 400 g of crushed ice and 300 g of potassium carbonate with external cooling. 125 g more of potassium carbonate is added, and the suspension is filtered. The cake is washed with around 11 of diethyl ether. The filtrate layers are separated, the ethereal layer is dried, filtered off and concentrated to give 2.9 g (30% yield) of a yellow oil (M+1=169) (purity #80%, used with no further purification).

1. temperaturecooling
2. stirringThe mixture is stirred at 80° C. for 2.5 hours
3. temperaturecooled down
4. filtrationthe suspension is filtered
5. washThe cake is washed with around 11 of diethyl ether
6. customThe filtrate layers are separated
7. customthe ethereal layer is dried
8. filtrationfiltered off
9. concentrationconcentrated