反应详情

温度

117 °C

Potassium methoxide (103 mg), lithium methoxide (27 mg) and tert-butanol (40 μl) were added to a solution of 5-bromo-4-chloro-1H-pyrrolo[2,3-b]pyridine (81 mg) in xylene (3.5 ml), and the mixture was heated under reflux at 117° C. for 16 hours. The reaction solution was brought to pH 4 by adding concentrated hydrochloric acid in small portions and separated by adding ethyl acetate and distilled water. The resulting aqueous layer was brought to pH 8 by adding a 5 N aqueous sodium hydroxide solution and separated by adding ethyl acetate. All the resulting organic layers were combined, washed with brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The resulting residue was purified by thin-layer chromatography (developed with ethyl acetate-hexane) to give the title compound (20 mg).

1. temperaturethe mixture was heated
2. customseparated
3. additionby adding ethyl acetate
4. distillationdistilled water
5. additionby adding a 5 N aqueous sodium hydroxide solution
6. customseparated
7. additionby adding ethyl acetate
8. washwashed with brine
9. dry with materialdried over anhydrous sodium sulfate
10. customThe solvent was evaporated under reduced pressure
11. customThe resulting residue was purified by thin-layer chromatography (developed with ethyl acetate-hexane)