反应详情

温度

60 °C

A solution of 2,3-dichlorofuro[2,3-c]pyridin-7-amine (5.7 g, 28.2 mmol) in MeCN (200 mL) was treated with N-iodosuccinimide (9.57 g, 42.3 mmol), added portionwise over 5-10 min. The mixture was heated at 60° C. for 16 h. After cooling to RT, the reaction was quenched with 20% aqueous sodium thiosulfate and stirred for 10 min. EtOAc (200 mL) was added and the phases separated. The organic phase was washed with 20% aqueous sodium thiosulfate (50 mL), then water (2×100 mL) and finally with brine. After drying over Na2SO4, the organic extracts were filtered and concentrated in vacuo. The material was purified using flash chromatography eluting with 2% MeOH in DCM to afford 3.8 g (41%) of the title compound. 1H NMR (300 MHz, DMSO-d6): δ 6.75 (br. s, 2H); 8.02 (s, 1H).

1. additionadded portionwise over 5-10 min
2. temperatureAfter cooling to RT
3. customthe reaction was quenched with 20% aqueous sodium thiosulfate
4. additionEtOAc (200 mL) was added
5. customthe phases separated
6. washThe organic phase was washed with 20% aqueous sodium thiosulfate (50 mL)
7. dry with materialAfter drying over Na2SO4
8. filtrationthe organic extracts were filtered
9. concentrationconcentrated in vacuo
10. customThe material was purified
11. washeluting with 2% MeOH in DCM