Dimethylformamide → HCID 12785887, compound

Participants

Reaction Steps

1 g of sodium bicarbonate and 0.8 g of hydroxylammonium chloride are added to 3 g of 7-bromo-5-(2-pyridyl)-1,3-dihydro-2H-1,4-benzodiazepine-2-thione in 60 ml of dioxane containing dimethylformamide and the mixture is stirred for 8 hours. 0.3 g of sodium bicarbonate and 0.25 g of hydroxylammonium chloride are again added and the mixture is stirred for 30 minutes at 50° C. The mixture is filtered off under suction when cold, and 1.0 ml of phenylisocyanate is added to the filtrate which is stirred for 1 hour. After the usual working up process, 1.6 g of colorless crystals are precipitated and are recrystallized from ethanol. Melting point 190° to 192° C.

Provenance & Evidence