Phosphorus oxychloride → HCID 10309275, compound

Participants

Reaction Steps

To an oven-dried round bottom flask fitted with a condenser was added the product of Step C (0.350 g; 0.986 mmol) and excess phosphorous oxychloride (1 mL). The reaction mixture was heated to reflux for 16 hours. The reaction mixture was allowed to cool to room temperature, and the volatiles were removed in vacuo. The residue was dissolved in ethyl acetate and washed with saturated NaHCO3 solution (2×), water, brine, dried (Na2SO4), filtered, and concentrated in vacuo. Purification was done by MPLC (silica gel; 0-10% ethyl acetate:hexane) to afford 0.283 g of the desired product: m/e=375 (M+2) Rt=4.36 min on LCMS.

Provenance & Evidence