| 摘要 |
<p>1,254,148. Purification of cephaloglycin. ELI LILLY & CO. 19 Nov., 1969 [17 Feb., 1969], No. 56685/69. Heading C2A. Cephaloglycin antibiotic [7-(D-α-aminophenyl. acetamido)cephalosporanic acid] is purified by (a) dissolving crude cephaloglycin with the aid of acid in a solvent mixture, (b) adding a base to the cephaloglycin solution in a quantity sufficient to precipitate cephaloglycin from the solution, and (c) separating the precipitated cephaloglycin from the base-treated solvent, the solvent mixture being an alkanenitrile (especially acetonitrile), a C 1-6 alkanol (especially methanol) and water with the alkanol being an optional part of step (a), said alkanol not used in step (a) being added as part of step (b) with the base, the proportions of alkanenitrile : alkanol : water in the solvent mixture being from 3 : 1 : 3 to 3 : 3 : 1 to 1 : 3 : 3 by volume. The process preferably also includes mixing the precipitated cephaloglycin from step (c) with water to form a crystalline cephaloglycin dihydrate. Preferably, in step (a), the solvent mixture comprises acetonitrile, methanol, and water in substantially equal parts by volume and hydrochloric acid is used to effect solution of the cephaloglycin in the solvent mixture. The base used may be ammonium, sodium or potassium hydroxide or a C 1-3 trialkylamine. The crude cephaloglycin starting material may be prepared by acylating 7-aminocephalosporanic acid with an N-blocked amino mixed anhydride form of phenylglycine and removing the N-protecting group. The purified cephaloglycin and the dihydrate formed therefrom may be used for forming aqueous solutions and suspensions for antibiotic therapy. Reference has been directed by the Comptroller to Specification 985,747.</p> |
