Sulfuric acid magnesium salt (1:1) → HCID 13649559, compound

Participants

Reaction Steps

To a suspension of 3 g of 3-(2-pyridinyl)-9H-pyrrolo[2,1-c]-1,2,4-triazolo[4,3-a][1,4]benzodiazepine in 50 mL of tetrahydrofuran is added 1.8 g of N-bromosuccinimide. The reaction mixture is allowed to stir at room temperature for 3 hours during which time a heavy white precipitate forms. A solution of aqueous sodium bisulfite is added to the reaction mixture and, after stirring for an additional 1 hour, the solid is collected and washed with 100 ml of water. The filtrate is evaporated to dryness under reduced pressure to yield a white solid. The combined solids are dissolved in 150 mL of methylene chloride, the solution is drived over anhydrous magnesium sulfate, filtered, and the solvent is evaporated under reduced pressure to yield 11-bromo-3-(2-pyridinyl)-9H-pyrrolo[2,1-c]-1,2,4-triazolo[4,3-a][1,4]benzodiazepine, m.p. 228°-229° (d). Product is recrystallized from a mixture of methylene chloride and diethyl ether.

Provenance & Evidence