反应详情

温度

130 °C

30 ml of cyclopropanecarboxylic acid and 70 ml of phosphoric acid (85%) were added to 15 g of 2,3-diamino-4-methylpyridine, and the mixture was stirred at an internal temperature of 130° C. for 12 hr. The reaction mixture was cooled, poured into a solution of 140 g of potassium hydroxide in 420 ml of water and then extracted with chloroform. The extract was dried over anhydrous magnesium sulfate and then concentrated. The residue was purified by column chromatography (chloroform:ethanol=97:3). The yield was 14.1 g, and the product was recrystallized from ethyl acetate-isopropyl ether to prepare the title compound in a pure form having a melting point of 203° to 204° C.

1. temperatureThe reaction mixture was cooled
2. extractionextracted with chloroform
3. dry with materialThe extract was dried over anhydrous magnesium sulfate
4. concentrationconcentrated
5. customThe residue was purified by column chromatography (chloroform:ethanol=97:3)
6. customThe yield was 14.1 g, and the product was recrystallized from ethyl acetate-isopropyl ether
7. customto prepare the title compound in a pure form