反应详情

温度

-78 °C

Under nitrogen atmosphere and ice cooling, to a solution of 11.1 g of N,N-diisopropylamine in 100 mL of tetrahydrofuran was added 66 mL of 1.6 M n-butyllithium in n-hexane and stirred at this temperature for 20 minutes. After cooling to −78° C., 15 mL of a solution containing 13.9 g of 2,4-difluorobenzonitrile in tetrahydrofuran was added dropwise. After stirring at this temperature for 10 minutes, 8.6 mL of N,N-dimethylformamide was added dropwise and stirred at this temperature for 15 minutes. The reaction solution was added with 20 mL of glacial acetic acid, followed by 200 mL water, and extracted twice with diethyl ether. The organic layer was washed successively with 0.2N hydrochloric acid and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated, and the resultant crude crystals were triturated with diethyl ether n-hexane, to afford 8.61 g of the title compound as bright yellow crystals.

1. additionwas added dropwise
2. stirringAfter stirring at this temperature for 10 minutes
3. stirringstirred at this temperature for 15 minutes
4. extractionextracted twice with diethyl ether
5. washThe organic layer was washed successively with 0.2N hydrochloric acid and saturated brine
6. dry with materialdried over anhydrous magnesium sulfate
7. customThe solvent was evaporated
8. customthe resultant crude crystals were triturated with diethyl ether n-hexane