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 1 l 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 1 l of diethyl ether
6. customThe filtrate layers are separated
7. customthe ethereal layer is dried
8. filtrationfiltered off
9. concentrationconcentrated