反应详情

5-fluoro-2-(methoxycarbonyl)pyridine 1-oxide (100 mg, 0.584 mmol) was dissolved in POCl3 (2 ml), and then heated at reflux under nitrogen stream for 4 hours. The resulting reaction liquid was slowly added to ice (15 g), and then extracted with MC (30 ml×2). The organic layer was dried over anhydrous sodium sulfate, followed by filtration and concentration, and then the residue thus obtained was subjected to MPLC (20% EtOAc/Hexanes), to obtain 88 mg of white solid (79%).

1. temperatureheated
2. temperatureat reflux under nitrogen stream for 4 hours
3. customThe resulting reaction liquid
4. extractionextracted with MC (30 ml×2)
5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
6. filtrationfollowed by filtration and concentration
7. customthe residue thus obtained