Methane → HCID 54001000, compound

Participants

Reaction Steps

3.957 g (8.14 millimol) of 3-chloro-4-[[4-[4-(diethylamino)-butyl]-1-piperidinyl]acetyl ]-1-methyl-1,4,9,10-tetrahydropyr rolo[3,2-b][1,5]benzodiazepin- 10-one were dissolved in 350 ml of hot ethanol and after the addition of 3 g of palladium on animal charcoal (20%), hydrogenated for 20 hours under a hydrogen pressure of 50 bar and at a temperature of 40° C. The catalyst was filtered off, the filtrate was concentrated by evaporation in vacuo, the crystalline hydrochloride was taken up in 20 ml of water, the solution obtained was made alkaline with sodium hydroxide and extracted exhaustively with dichloromethane. The combined extracts were dried over sodium sulphate and evaporated down and the residue remaining was recrystallised. 1 g (26.3% of theory) of colourless crystals were obtained, m.p. 198° C. (acetonitrile).

Provenance & Evidence