反应详情

温度

55 °C

Di-tert-butyl (2-chloro-3-methylfuro[2,3-c]pyridin-7-yl)imidodicarbonate (3.2 g, 8.38 mmol) DCM (25 mL) was cooled in an ice bath and treated with 4 N HCl in 1,4-dioxane (12.5 mL, 50 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 and the residue was suspended in DCM and treated with saturated NaHCO3 until the pH reached ˜8.5. The organic layer was washed with water, then brine and then dried over anhydrous Na2SO4. After concentration in vacuo, the material was purified by flash chromatography (3% MeOH:DCM) to provide 1.0 g (66%) of the title compound. 1H NMR (400 MHz, CDCl3) δ 7.87 (d, J=5.4 Hz, 1H), 6.79 (d, J=5.4 Hz, 1H), 4.78 (br s, 2H), 2.16 (s, 3H).

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
6. dry with materialbrine and then dried over anhydrous Na2SO4
7. concentrationAfter concentration in vacuo
8. customthe material was purified by flash chromatography (3% MeOH:DCM)