Phosphorus trichloride → HCID 70505024, compound

Participants

Reaction Conditions

Reaction Steps

A 41.5 ml portion of PCl3 was added to a solution of 32 g of diphenylmethyl 7-(2-thienylacetamido)-2-methyl-3-acetoxymethylceph-3-em-4-carboxylate 1-oxide in 200 ml of DMF at -50° C., and the mixture was stirred at -30° C. for 5 minutes and poured in ice water to extract with AcOEt. The AcOEt layer was washed with 5% aqueous NaHCO3 and saturated aqueous sodium chloride solutions, and dried over Na2SO4, followed by distilling off the AcOET under reduced pressure, thus yielding crude crystals. Recrystalization from AcOEt-Et2O (1:3) afforded 17 g (55%) of diphenylmethyl 7-(2-thienylacetamido)-2β-methyl-3-acetoxymethylceph-3-em-4-carboxylate.

Provenance & Evidence