Hydrochloric Acid → HCID 19085168, compound

Participants

Reaction Conditions

Reaction Steps

Ethyl 2-(4-(2-chlorophenyl)-2-ethyl-9-methyl-6H-thieno[3,2-f] [1,2,4]triazolo[4,3-a] [1,4]diazepin-6-yl)acetate (1.0 g) synthesized by a known method such as WO94/06802 was added to 2M hydrochloric acid (24 ml), and the mixture was stirred at 60° C. for 0.5 hour. The reaction mixture was cooled to 0° C. A saturated aqueous sodium hydrogencarbonate solution, chloroform and 3,4-dichlorobenzoyl chloride (0.53 g) were added and the mixture was stirred for 1 hour. The organic layer was taken out and dried over magnesium sulfate. The residue was purified by silica gel column chromatography (developing solvent:ethyl acetate-hexane) and crystallized from diisopropyl ether to give 0.06 g of ethyl 3-(4-(3-(2-chlorobenzoyl)-5-ethylthiophen-2-yl)-5-methyl[1,2,4]triazol-3-yl)-3-(3,4-dichlorobenzoylamino)propionate.

Provenance & Evidence