反应详情

温度

80 °C

The crude 5-nitro-2-trifluoromethyl-pyridin-4-ol (3.4 g, 16.3 mmmol) was treated with PCl5 (5.2 g, 24.97 mmol) and POCl3 (7 mL, 24.49 mmol). The resulting mixture is heated at 80° C. for 18 h, cooled and poured into ice-cold water, and extracted with CH2Cl2. The combined organic phase is washed successively with saturated aqueous NaHCO3, water, brine, dried over Na2SO4, and concentrated in vacuo to afford 4-Chloro-5-nitro-2-trifluoromethyl-pyridine as an yellow oil. 1H NMR (300 MHz, CDCl3): δ 9.17 (s, 1H), 7.9 (s, 1H).

1. temperaturecooled
2. additionpoured into ice-cold water
3. extractionextracted with CH2Cl2
4. washThe combined organic phase is washed successively with saturated aqueous NaHCO3, water, brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated in vacuo