Methanol → HCID 67894757, compound

Participants

Reaction Steps

To a suspension of phorphorus pentachloride (624 mg) in methylene chloride (15 ml) was added pyridine (0.242 ml) at -20° C. After the mixture was stirred for 20 minutes at the same temperature, p-nitrobenzyl 7-(2-phenylacetamido)-3-chloromethyl-3-cephem-4-carboxylate (502 mg) was added to the mixture at -20° C. The mixture was stirred for 30 minutes under ice-cooling. To the mixture was added methanol (0.65 ml) at -20° C., and the mixture was stirred for an hour at -20°~-5° C. Water (0.7 ml) was added thereto under ice-cooling. The mixture was stirred for an hour at the same temperature to give a precipitate. The precipitate was collected, washed with methylene chloride, water and diisopropyl ether successively and dried over phosphorus pentoxide to give p-nitrobenzyl 7-amino-3-chloromethyl-3-cephem-4-carboxylate monohydrochloride (0.35 g).

Provenance & Evidence