Benzenesulfonyl chloride → HCID 178481967, compound

Participants

Reaction Steps

To an ice cold stirred solution of 0.388 g. (0.0022 mole) of benzenesulfonyl chloride in 15 ml. of dried pyridine, 0.721 g. (0.002 mole) of 1-amino-8-chloro-3-methyl-6-phenyl-4H-s-triazolo[4,3-a][1,4]benzodiazepinium chloride (VI) is added. The resulting mixture is kept in an ice bath for about 15 hours and then allowed to warm to room temperature and stand for about 6 hours. It is then poured into cold, dilute aqueous sodium bicarbonate solution and extracted with chloroform. The extract is washed with brine, dried with sodium sulfate and concentrated. The residue is crystallized to give 1-benzenesulfonamido-8-chloro-3-methyl-6-phenyl-4H-s-triazolo[4,3-a][1,4]benzodiazepinium hydroxide inner salt (X).

Provenance & Evidence