Phosphoric Acid → HCID 88839754, compound

Participants

Reaction Steps

To a stirred solution of 5.4 g. (0.02 mole) of 7-aminocephalosporanic acid and 3.36 g. (0.04 mole) of sodium bicarbonate in 120 ml. of aqueous phosphate buffer (pH 6.4) was added 3.1 g. (0.02 mole) of 4-methylthiazole-2-thiolcarboxylic 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 phosphorous pentoxide 3.75 g. of crystalline yellow solid. Yield = 50.5% NMR spectrum was consistent with the structure of the title product.

Provenance & Evidence