反应详情

100 mg (0.76 mmol) of 1H-pyrrolo[2,3-b]pyridine 7-oxide (from example XV) in 3 ml of phosphorus oxychloride are heated at reflux until a clear solution is formed. After cooling to room temperature, the reaction mixture is carefully hydrolyzed with ice. The mixture is made alkaline using ammonia and extracted repeatedly with ethyl acetate. The organic phase is washed with water and saturated sodium chloride solution. After drying over magnesium sulfate, the solvent is removed under reduced pressure. This gives a yellow oil which is purified by preparative HPLC.

1. temperatureat reflux until a clear solution
2. customis formed
3. extractionextracted repeatedly with ethyl acetate
4. washThe organic phase is washed with water and saturated sodium chloride solution
5. dry with materialAfter drying over magnesium sulfate
6. customthe solvent is removed under reduced pressure
7. customThis gives a yellow oil which
8. customis purified by preparative HPLC