Oxalic Acid → HCID 178482830, compound

Participants

Reaction Conditions

Reaction Steps

In 1430 ml of 95% aqueous ethanol solution was dissolved 239 g of N-[2-(4-carbamoylphenyl)-2hydroxyethyl]-N'-methanesulfonyl-N"-[2-[[5-(methylamino)methyl-2-furyl]methylthio]ethyl]guanidine. Thereto was added a solution formed by dissolving 46.8 g of oxalic acid in 240 ml of 95% aqueous ethanol solution. Further, 2.5 g of a seed crystal was added thereto. The mixture was stirred at 40° C. for 3 hours and at room temperature for 3 hours and then allowed to stand overnight. The crystals deposited were collected by filtration to obtain 257 g (yield: 91%) of N-[2-(4-carbamoylphenyl)-2-hydroxyethyl]-N'-methanesulfonyl-N"[2-[[5-(methylamino)methyl-2-furyl]methylthio]ethyl]guanidine oxalate (1:1). Melting point: 142.5°-145.5° C. (recrystallized from 95% aqueous ethanol solution)

Provenance & Evidence