Example 1
To a vial containing the SM (83 mg, 0.291 mmol) and DCE (1.45 mL) was added POCl3 (0.136 mL, 1.45 mmol). The reaction mixture was stirred at 90 C overnight. The mixture was quenched by pouring into ice-H2O, then extracted with EtOAc. The layers were separated and the aq layer was further extracted with EtOAc. The combined organics were dried (Na2SO4) and concentrated to provide the product as a light yellow solid that was taken forward without further purification.
[Patent Reference: WO2014201173, page 75, (19.7 MB)]