HCID 13389345, compound → HCID 178515278, compound

Participants

Reaction Steps

In an inert atmosphere, 6 g of the product of Step A were mixed with 60 ml of anisole and the insoluble matter was removed by filtering. 2.4 ml of phenyl hydrazine were added to the filtrate and the mixture was placed in a water bath at 150° C. for 21/2 hours. The mixture was cooled, dried, washed with ethyl acetate and evaporated to dryness. The residue was washed with an aqueous solution of N hydrochloric acid and was dissolved in a solution of 25 ml of concentrated ammonia and 75 ml water. The solution was filtered and the aqueous phase was extracted with ether. Sodium phosphate was added and the product was purified by triturating in ethanol, then in water. The product was dried to obtain 2.22 g of 8-chloro-2,5-dihydro-2-phenyl-3H-pyrazolo[4,3-c]cinnolin-3-one melting at >280° C.

Provenance & Evidence