Diethyl chlorophosphate → HCID 10097974, compound

Participants

Reaction Steps

To a suspension of 4-[4-chloro-5-(4-ethoxyphenyl)imidazol-1-yl]benzenesulfonamide sodium salt (2.89 mmol) (obtained in the preceding section) in THF (12 mL), diethyl chlorophosphate (0.42 mL, 2.89 mmol) was added under argon atmosphere. The resulting solution was stirred at room temperature for 15 days. It was then concentrated to dryness and the resulting residue was partitioned between H2O and EtOAc, the suspension was filtered and the phases separated. The organic phase was dried and concentrated to afford a solid which was purified by chromatography on silica gel using mixtures hexane/EtOAc and EtOAc/MeOH of increasing polarity as eluent. The product obtained was then recrystallized from ACN to afford the title compound of the example as a yellowish solid (15% yield).

Provenance & Evidence