Antimony pentachloride → 7-Amino-3-methoxymethyl-3-cephem-4-carboxylic acid

Participants

Reaction Conditions

Reaction Steps

To 15 ml of sulfolane were added 2.72 g of 7-ACA, 2.3 g of methanol, 2.8 g of antimony pentachloride and 12 g of bismuth trichloride. The mixture was heated at 50° C. for 40 min to advance a reaction. After completion of the reaction, the reaction mixture was cooled to 5° C. The resulting precipitate was filtered off To the filtrate was added 60 ml of water, and then the resulting mixture was stirred homogeneously. To the resulting solution was added 0.5 g of activated carbon, and then the mixture was stirred, followed by filtration. The filtrate was adjusted to pH 3.5 with sodium bicarbonate. To the resulting mixture was added 30 ml of methanol, thereby to form a white crystalline precipitate. The white crystalline precipitate was collected by filtration, and washed with 10 ml of cold water and, then, with 10 ml of cold methanol to obtain the desired product, namely 7-amino-3-methoxymethyl-3-cephem-4-carboxylic acid. The amount of the desired product was 1.29 g. The yield of the desired product was 53 %. .

Provenance & Evidence