Chloroform → HCID 19085262, compound

Participants

Reaction Conditions

Reaction Steps

4-(2-Chlorophenyl)-2-(2-(4-isobutylphenyl)ethyl)-9-methyl-6H-thieno[3,2-f] [1,2,4]triazolo[4,3-a] [1,4]diazepine described in Example 1 of Japanese Patent Publication No. 55510/1993 was dissolved in a 5% aqueous hydrochloric acid solution, and the solution was stirred at 60° C. for 5 hours. A saturated aqueous sodium hydrogencarbonate solution was added to the reaction mixture to make the mixture alkaline. Chloroform and 3,4-dichlorobenzoyl chloride were added, and the mixture was stirred under ice-cooling for 1 hour. The organic layer was washed with an aqueous citric acid solution, a saturated aqueous sodium hydrogencarbonate solution and saturated brine, and dried over magnesium sulfate. The solvent was evaporated, and the residue was purified to give N-(4-(3-(2-chlorobenzoyl)-5-(2-(4-isobutylphenyl)ethyl)thiophen-2-yl)-5-methyl[1,2,4]triazol-3-ylmethyl)-3,4-dichlorobenzamide.

Provenance & Evidence