2,2'-Bipyridine → HCID 51349325, compound

Participants

Reaction Conditions

Reaction Steps

3-(3-cyano-4-hydroxy-5-iodobenzoyl)-1,1-dioxo-2,3-dihydro-1,3-benzothiazole (500 mg) was dissolved in N,N-dimethylformamide (5 mL), and 2,2′-bipyridine (18 mg), zinc powder (149 mg), nickel bromide (25 mg) and diethyl disulfide (70 mg) were added to the solution, and then the mixture was stirred at 110° C. for 1 hour. After the reaction solution was filtered, 1N hydrochloric acid was added and the reaction mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the obtained residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1) and then crystallized from diethylether-ethyl acetate to obtain the title compound (63 mg) as a colorless crystal.

Provenance & Evidence