反应详情

To a 50 mL flask was added 10 (221 mg, 1 mmol) and 10 mL POCl3. The resulting mixture was refluxed for 2 h, and the solvent was removed under reduced pressure to afford a dark residue. To this was added mL of CHCl3 and 300 mg of silica gel. The solvent was evaporated to afford a plug. Column chromatography of the plug with hexane: acetyl acetate=20:1 as eluent afford 105 mg (44%) of 11 as a yellow solid:

1. temperatureThe resulting mixture was refluxed for 2 h
2. customthe solvent was removed under reduced pressure
3. customto afford a dark residue
4. customThe solvent was evaporated
5. customto afford a plug