反应详情

Ethyl-4-amino-7-bromo-5-(4-nitrophenyl)pyrrolo[2,1-f][1,2,4]triazine-6-carboxylate (2.06 g, 5.07 mmol) was suspended in EtOH (30 mL) and treated with tin(II)chloride dihydrate (3.66 g. 16.2 mmol). The mixture was heated to reflux for 18 h. The mixture was concentrated then diluted with EtOAc and saturated NaHCO3 solution. The emulsion was filtered and the filtrate was transferred to a separatory funnel. The organic layer was washed with water and saturated NaCl solution, dried then (MgSO4) and concentrated to afford 1.5 g of the desired product as tan solid (79%). 1H-NMR (DMSO-d6) δ 8.00 (s, 1H), 7.00 (d, J=8.6, 1H), 6.62 (d, J=9.2, 3H), 5.40 (bd, 2H), 5.19 (bs, 2H), 4.05 (q, J=7.0, 2H), 1.03 (t, J=7.0, 3H); MS [M+H]+=376.0, 378.0; LCMS RT=2.02.

1. temperatureThe mixture was heated
2. temperatureto reflux for 18 h
3. concentrationThe mixture was concentrated
4. additionthen diluted with EtOAc and saturated NaHCO3 solution
5. filtrationThe emulsion was filtered
6. customthe filtrate was transferred to a separatory funnel
7. washThe organic layer was washed with water and saturated NaCl solution
8. customdried
9. concentration(MgSO4) and concentrated