反应详情

温度

100 °C

To a solution of tert-butyl 2-cyano-2-(5-nitro-3-(trifluoromethyl)pyridin-2-yl)acetate (7 g, 21.13 mmol) in MeOH (100 mL) was added aqueous HCl (40 mL, 1316 mmol). The resulting mixture was stirred at 100° C. overnight. After TLC analysis (PE/EA=10/1) showed the starting material was consumed, the solvent was removed in vacuo. The residue was dissolved in H2O (50 mL) and extracted by EA (100 mL). The organic layer was washed with aqueous NaHCO3 and brine and then dried over Na2SO4. After filtration, the filtrate was concentrated to give the crude product, which was purified by column chromatography (PE/EA=10/1) to yield a brown solid of 2-(5-nitro-3-(trifluoromethyl)pyridin-2-yl)acetonitrile (4.3 g, 17.77 mmol, 84% yield): 1H NMR (400 MHz, CD3OD) δ 9.59 (s, 1H), 8.88 (d, J=2.4 Hz, 1H), 4.86 (s, 2H); ES-LCMS m/z: 232.1 (M+H).

1. customwas consumed
2. customthe solvent was removed in vacuo
3. dissolutionThe residue was dissolved in H2O (50 mL)
4. extractionextracted by EA (100 mL)
5. washThe organic layer was washed with aqueous NaHCO3 and brine
6. dry with materialdried over Na2SO4
7. filtrationAfter filtration
8. concentrationthe filtrate was concentrated
9. customto give the crude product, which
10. customwas purified by column chromatography (PE/EA=10/1)