Sodium Hydroxide → HCID 12472016, compound

Participants

Reaction Steps

10-Chloro-3-(chloromethyl)-7-methyl-5H-s-triazolo[4,3-d][1,4]benzodiazepin-6(7H)-one (5 g, prepared as described in Example 9) is suspended in 50 ml of 1,2-dimethoxyethane. N-methylpiperazine (5.4 g) is added to the suspension and the mixture is heated under reflux for 5 hours. The solvent is stripped off, 3N aqueous sodium hydroxide is added to the residue and the mixture is extracted with several portions of chloroform. The combined chloroform extracts are dried over sodium sulfate and the solvent is removed under vacuum to leave a residue which is recrystallized from absolute ethanol to yield 4 g of the title compound, melting point 228.5°-230.5° C.

Provenance & Evidence