1,2-Dichlorobenzene → HCID 178428634, compound

Participants

Reaction Conditions

Reaction Steps

125 g of 3-aminocrotonitrile were introduced into 250 ml of anhydrous o-dichlorobenzene and stirred at 100° C. To this were added 233 g of N-cyanoacetyl-N'-phenoxyacetylhydrazine a little at a time, and the mixture was then stirred at 140° C. for 2 hours. 120 g of acetic anhydride were added and the mixture was then refluxed for 2 hours and, while cooling, 500 ml of methanol were added. After cooling, the precipitate was filtered off with suction, washed with methanol and dried at 80° C. under reduced pressure. 213 g of 6-cyano-7-hydroxy-5-methyl-2-phenoxymethyl[1,2,4]triazolo[2,3-a]-pyridine were obtained as a colorless powder. A sample recrystallized from γ-butyrolactone does not melt up to 350° C. and has the following analysis:

Provenance & Evidence