Potassium Carbonate → HCID 19881116, compound

Participants

Reaction Steps

To a solution of 5.0 g of 5-(4-chlorobutyl)-5,6,7,8-tetrahydro-2-methyl-4H-thieno[3,2-c]azepin-4-one in 60 ml of acetic acid was added 1.9 ml of bromine at 60° C. and stirred for 20 minutes. After cooling, to the mixture was added an aqueous saturated sodium thiosulfate solution and the mixture was neutralized with potassium carbonate, and then extracted with ethyl acetate. The extract was washed with water, dried and concentrated under reduced pressure. The resulting crude crystals were recrystallized from a mixed solvent of isopropyl alcohol and hexane to give 2.3 g of 3-bromo-5-(4-chlorobutyl)-5,6,7,8-tetrahydro-2-methyl-4H-thieno[3,2-c]azepin-4-one as pale yellow crystals, melting at 78°-80° C.

Provenance & Evidence