Diethylene Glycol → HCID 21393430, compound

Participants

Reaction Conditions

Reaction Steps

800 mg (0.00285 mol) 2-methyl-10-oxo-1,2,3,4,10,14b-hexahydro-benzo[c]pyrazino[1,2-a]pyrido[3,4-f]azepine is added to a well-stirred suspension consisting of 4 ml di-ethylene glycol, 1 ml DMSO, 0.4 g KOH and 1 ml 80% hydrazine hydrate. The reaction is exothermic; the temperature of the reaction mixture is adjusted to 120° C and held there for 30 minutes. During this period hydrazine/water (0.8 ml) is distilled off, and the reaction temperature is then raised to 160° C for 2 hours. The reaction mixture is subsequently cooled, poured into water, and extracted with ether. After drying, and removing the solvent by evaporation, 685 mg (90%) 2-methyl-1,2,3,4,10,14b-hexahydro-benzo[c]pyrazino[1,2-a]pyrido[3,4-f]azepine is obtained as a light yellow oil.

Provenance & Evidence