Phosphorus pentachloride → HCID 53839116, compound

Participants

Reaction Steps

240 g (1 mol) of thien-2-yl-glyoxylic acid ethyl ester 2-acetylhydrazone were dissolved in 1,000 ml of methylene chloride and 208 g (1 mol) of phosphorus pentachloride were added at -10° to 0° C. Stirring was continued for half an hour, ice-water was added to the reaction mixture and the batch was neutralised with sodium bicarbonate solution. The organic phase was separated off, dried over sodium sulphate and concentrated by distilling off the solvent. 234 g (0.92 mol) of crude 1-ethoxycarbonyl-4-chloro-4-methyl-1-thien-2-yl-2,3-diazabutadiene were obtained as an oil which would be directly reacted further. ##STR11##

Provenance & Evidence