反应详情

HCl gas is bubbled through a solution of 6-chloro-1H-pyrrolo[2,3-b]pyridine-2-carboxylic acid (36 g, 183 mmol) in ethanol (500 mL) at 0° C. for 30 min. The reaction mixture is then heated at reflux for 16 h. The solvent is evaporated and the residue is diluted with CH2Cl2 and filtered. The filtrate is evaporated and the residue is washed with diethyl ether (2×250 mL). The organic layers are dried (Na2SO4) and concentrated. The crude residue is purified by passing through the column of neutral alumina, eluting with 10% EtOAc/hexane to afford the title compound as a white solid (10 g, 25%).

1. temperatureThe reaction mixture is then heated
2. temperatureat reflux for 16 h
3. customThe solvent is evaporated
4. additionthe residue is diluted with CH2Cl2
5. filtrationfiltered
6. customThe filtrate is evaporated
7. washthe residue is washed with diethyl ether (2×250 mL)
8. dry with materialThe organic layers are dried (Na2SO4)
9. concentrationconcentrated
10. customThe crude residue is purified
11. washeluting with 10% EtOAc/hexane