Phosphorus oxychloride → HCID 18520070, compound

Participants

Reaction Steps

A suspension of Example 137 A (4.50 g; 19.0 mmol) in phosphoryl chloride (50 ml) is heated to reflux temperature in the course of 1.5 h and stirred at this temperature overnight. The phosphoryl chloride is stripped off in vacuo, the residue is treated with ice water and the mixture is extracted with dichloromethane. The organic phase is washed with sat. NaHCO3 solution, dried (Na2SO4) and concentrated in vacuo. The residue is chromatographed on silica gel using toluene:EA (5:1).

Provenance & Evidence