Carbon Tetrachloride → HCID 66941854, compound

Participants

Reaction Steps

In carbon tetrachloride (100 ml), 5-methyl-benzo[b]thiophene-2-carboxylic acid ethyl ester (2.36 g) prepared by the method described in PCT Patent WO 0153291 was dissolved. The solution was added with N-bromosuccinimide (2.00 g) and azobisisobutyronitrile (140.7 mg), and the whole was stirred for 17 hours under thermal reflux. After the insoluble matter had been removed through filtration, the residue was recrystallized with methanol. Then, the crystal was dissolved in DMF (20 ml) and then added with potassium phthalimide (1.18 g), followed by stirring overnight at room temperature. After the solvent had been distilled off, the residue was added with water and extracted with chloroform. The organic layer was washed with saturated saline solution and dried with anhydrous sodium sulfate, thereby obtaining the subject compound (1.15 g) as a pale-yellow solid.

Provenance & Evidence