Picolinohydrazide → HCID 23317235, compound

Participants

Reaction Steps

Under an atmosphere of nitrogen, a slurry of 575 g of 11-chloro-5H-pyrrolo[2,1-c][1,4]benzodiazepine in 7.2 L of anhydrous ethanol is stirred while 364 g of pyridine-2-carboxylic acid hydrazide is added over a period of five minutes. The mixture is heated slowly to 65°. An exothermic reaction occurs and there is vigorous refluxing. When the refluxing subsides to a normal rate heating is continued and the mixture is stirred and refluxed for 21-22 hours. The product precipitates from the hot solution during the reflux period. The crystals are filtered off and washed on the filter with anhydrous ethanol. The product is air-dried overnight, then dried at high vacuum without heat for 2 days to yield 3-(2-pyridinyl)-9H-pyrrolo[2,1-c]-1,2,4-triazolo[4,3-a][1,4benzodiazepine hydrochloride, m.p. 265°-268° (d).

Provenance & Evidence