反应详情

To a solution of 3.98 g. (0.02 mole) of 2-ethylamino-6-methylnicotinic acid methyl ester in 50 ml. of anhydrous diethyl ether was added 1.5 g. (0.01 mole) of ethyl malonyl chloride. The mixture was stirred at room temperature for 1 hour. The mixture was filtered and the filtrate was evaporated in a rotary evaporator. The residue was added to a solution of 0.23 g. of sodium in 50 ml. of absolute ethanol and was warmed for 5 minutes. The mixture was cooled and the insoluble material was collected and was dissolved in water. Acidification of the water solution with glacial acetic acid afforded a precipitate which was collected, air dried and was recrystallized from heptane to give 1.2 g. of product, m.p. 147°-151° C.

1. filtrationThe mixture was filtered
2. customthe filtrate was evaporated in a rotary evaporator
3. additionThe residue was added to a solution of 0.23 g
4. temperatureof absolute ethanol and was warmed for 5 minutes
5. temperatureThe mixture was cooled
6. customthe insoluble material was collected
7. dissolutionwas dissolved in water
8. customAcidification of the water solution with glacial acetic acid afforded a precipitate which
9. customwas collected
10. customair dried
11. customwas recrystallized from heptane
12. customto give 1.2 g