Methanol → HCID 131728254, compound

Participants

Reaction Steps

A 1.0 g quantity of 7-amino-3-[2-(4-methylthiazol-5-yl)vinyl]-3-cephem-4-carboxylic acid (E-isomer: 9% by HPLCb)) was suspended in a solvent mixture of 2 ml of water and 5 ml of methanol in a four-necked 100-ml flask. With addition of 0.68 ml of dicyclohexylamine, the suspension was stirred until crystals separated out from a transparent solution subsequently formed. The reaction mixture was allowed to stand at room temperature for 15 minutes and thereafter stirred for 15 minutes, and 7 ml of acetone was then slowly added to the mixture. The resulting mixture was subsequently cooled in an ice bath for 2 hours, and the resulting crystals were filtered off, washed with acetone and dried, affording 7-amino-3-[2-(4-methylthiazol-5-yl)vinyl]-3-cephem-4-carboxylic acid dicyclohexylamine salt. While the filtration treatment in Examples was completed in about 1 minute, the filtration procedure in this comparative example required about 10 minutes.

Provenance & Evidence