反应详情

温度

155 °C

A mixture of 2-(6-bromo-3,4-diethoxy-2-fluorobenzyl)isoindol-1,3-dione (1.00 g, 2.37 mol), copper cyanide (0.42 g, 4.74 mol) and N,N-dimethylformamide (5 mL) was stirred at 155° C. for ten hours. After the reaction mixture was extracted with a 10% aqueous solution of ethylene diamine and toluene, the resultant organic layer was washed sequentially with a 10% aqueous solution of ethylene diamine and saturated brine and dried over anhydrous sodium sulfate. After filtration, the solvent was distilled off to give crude crystals, which were washed with ethyl acetate to give 0.52 g of the title compound (yield: 60%) as slightly green crystals.

1. extractionAfter the reaction mixture was extracted with a 10% aqueous solution of ethylene diamine and toluene
2. washthe resultant organic layer was washed sequentially with a 10% aqueous solution of ethylene diamine and saturated brine
3. dry with materialdried over anhydrous sodium sulfate
4. filtrationAfter filtration
5. distillationthe solvent was distilled off
6. customto give crude crystals, which
7. washwere washed with ethyl acetate