反应详情

A mixture of stannous chloride dihydrate (41 g) and concentrated hydrochloric acid (40 ml) was added slowly to a solution of 2-methoxy-4-methyl-5-nitropyridine (5.1 g) in acetic acid (40 ml), maintaining the temperature below 35° C. The resulting mixture was stirred at room temperature for 2 hours, and then allowed to stand overnight in the refrigerator. The solid was collected and both solid and supernatant were separately basified with a 20% sodium hydroxide solution. The product was extracted with chloroform, combined, dried (anhydrous magnesium sulfate) and concentrated to give 3.9 g of the title compound as a solid, suitable for use in the next reaction.

1. temperaturemaintaining the temperature below 35° C
2. waitto stand overnight in the refrigerator
3. customThe solid was collected
4. extractionThe product was extracted with chloroform
5. dry with materialdried (anhydrous magnesium sulfate)
6. concentrationconcentrated