HCID 131717597, compound → HCID 131717596, compound

Participants

Reaction Steps

The said hydrochloride was suspended at 20° C. in 820 ml of 90% ethanol and the suspension was refluxed while 1 ml of 22° Be was added thereto. The mixture was filtered hot and the filter was rinsed with 41 ml of 90% ethanol. 25 ml of triethylamine were added with stirring over 15 minutes to the filtrate at 45° to 50° C. and the mixture was then stirred at 18° to 20° C. for 2 hours and was vacuum filtered. The product was washed 3 times with 83 ml of ethanol and 3 times with 82 ml of demineralized water and dried at 40° C. under reduced pressure to obtain 66 g (64.6 g on dry basis) of the syn isomer of 3-methyl-7-[2-(2-amino-4-thiazolyl)-2-methoxyimino-acetamido]-ceph-3-eme-4-carboxylic acid. A second yield of 4.7 g of the product was obtained under the same conditions for a total yield of 69.3 g (75.1% yield).

Provenance & Evidence