反应详情

温度

120 °C

5H-Furo[3,2-c]pyridin-4-one (5.9 g) was suspended with POCl3 (12 ml) and the reaction mixture was stirred for 3 hours at 120° C. After evaporating POCl3, crushed ice was added and poured into the mixture of ethyl acetate and saturated NaHCO3. The corresponding organic phase was separated and dried over Na2SO4 and then concentrated in vacuo. The resultant residue was purified by chromatography on a silica gel column to afford 4-chloro-furo[3,2-c]pyridine (5.6 g) 1H NMR (400 MHz, DMSO-d6) ppm 8.31 (d, J=5.8 Hz, 1H), 8.26 (d, J=2.3 Hz, 1H), 7.79 (dd, J=1.0, 5.6 Hz, 1H), 7.13 (dd, J=1.0, 2.3 Hz, 1H).

1. customAfter evaporating POCl3
2. customcrushed ice
3. additionwas added
4. additionpoured into the mixture of ethyl acetate and saturated NaHCO3
5. customThe corresponding organic phase was separated
6. dry with materialdried over Na2SO4
7. concentrationconcentrated in vacuo
8. customThe resultant residue was purified by chromatography on a silica gel column