Phosphoric Acid → HCID 88840158, compound

Participants

Reaction Steps

To a stirred solution of 7.22 g. (0.0265 mole) of 7-aminocephalosporanic acid and 4.45 g. (0.053 mole) of sodium bicarbonate in 160 ml. of aqueous phosphate buffer (ph 6.4) was added 4.6 g. (0.0265 mole) of 4,5-dimethylthiazole-2-thiolcarboxyic acid. The mixture was stirred in a nitrogen atmosphere and heated to 50°. The pH was adjusted from 7.0 to 6.5 with 42% phosphoric acid. A crystalline solid started to precipitate. After 5 hours at 50° the reaction mixture was cooled to 20°. The precipitated solid was collected by filtration, washed with water and acetone and dried in vacuo over phosphorus pentoxide to provide 4.55 g. of a tan crystalline material. Yield = 45%. NMR spectrum was consistent with structure.

Provenance & Evidence