反应详情

温度

80 °C

The general procedure was taken from Wang et al. Tetrahedron Lett. 2005, 46, 2631. To a solution of 1-(4-trifluoromethoxyphenyl)-pyrazolidin-3-one (120 mg, 0.49 mmol, 1.00 eq) in toluene (20 mL) was slowly added phosphoryl chloride (22.5 mg, 1.47 mmol, 3.00 eq). The mixture was then heated at 80° C. for 1 h before cooling to room temperature and quenching with H2O (10 mL). The vessel was stirred under an atmosphere of nitrogen (N2) for 8 h before the product was extracted into EtOAc (200 mL), dried (MgSO4), and concentrated under reduced pressure. GC-MS proved 88% formation of the desired intermediate, which was used in subsequent reactions without further purification.

1. temperaturebefore cooling to room temperature
2. customquenching with H2O (10 mL)
3. extractionwas extracted into EtOAc (200 mL)
4. dry with materialdried (MgSO4)
5. concentrationconcentrated under reduced pressure
6. customGC-MS proved 88% formation of the desired intermediate, which was used in subsequent reactions without further purification