反应详情

温度

-78 °C

Lithium diisopropylamide (2M in heptane/THF/benzene, 16.7 mL) was treated dropwise with 2,4-dichloropyridine (5 g, 33.8 mmol) at −78° C. in THF (25 mL). The mixture was stirred at −78° C. for 2 hours, treated with excess dry ice, allowed to warm up to room temperature, and partitioned between diethyl ether and an equal volume of 10% aqueous KOH. The basic extract was neutralized with 10% HCl and extracted with diethyl ether. The ethereal extract was dried (Na2SO4), filtered, and the filtrate wasconcentrated under reduced pressure to provide 9.5 g (70% yield) of the title compound. 1H NMR (300 MHz, DMSO-D6) δ ppm 3.32 (s, 1H), 7.74 (d, J=5.42 Hz,1H), 8.47 (d, J=5.42 Hz,1H).

1. temperatureto warm up to room temperature
2. custompartitioned between diethyl ether
3. extractionThe basic extract
4. extractionextracted with diethyl ether
5. extractionThe ethereal extract
6. dry with materialwas dried (Na2SO4)
7. filtrationfiltered