反应详情

温度

55 °C

Di-tert-butyl (2-chlorofuro[2,3-c]pyridin-7-yl)imidodicarbonate (18.0 g, 49.1 mmol) in DCM (100 mL) was cooled in an ice bath and treated with 4 N HCl in 1,4-dioxane (75 mL, 300 mmol) added slowly over several minutes. The reaction was removed from the cooling bath and heated at 55° C. for 16 h. The mixture was concentrated in vacuo. The residue was suspended in DCM and treated with saturated NaHCO3 until the pH reached ˜8.5. The organic layer was washed with water and brine and then dried over anhydrous Na2SO4. The material was purified by flash chromatography (50% EtOAc:DCM) to provide 8.2 g (100%) of the title compound as a white solid. 1H NMR (CDCl3, 400 MHz): δ 4.75 (br s, 2H), 6.54 (s, 1H), 6.85 (d, J=5.3 Hz, 1H), 7.86 (d, J=5.3 Hz, 1H); MS (ESI): 169.12 [M+H]+.

1. additionadded slowly over several minutes
2. customThe reaction was removed from the cooling bath
3. concentrationThe mixture was concentrated in vacuo
4. additiontreated with saturated NaHCO3 until the pH
5. washThe organic layer was washed with water and brine
6. dry with materialdried over anhydrous Na2SO4
7. customThe material was purified by flash chromatography (50% EtOAc:DCM)