Potassium Carbonate → HCID 86609946, compound

Participants

Reaction Steps

tert-Butyl (5-bromo-3,4-dimethyl-1,3-thiazol-2(3H)-ylidene)carbamate (2.9 g) obtained in Example 30b) was dissolved in 1,2-dichloroethane (50 mL). AIBN (0.1 g) and NBS (1.7 g) were added thereto at room temperature, and the mixture was mixed at 80° C. for 3 hours. The reaction solution was poured into an aqueous potassium carbonate solution. The mixture was extracted with chloroform, and the extract was dried over anhydrous magnesium sulfate. The solvent was distilled off to give tert-butyl (5-bromo-3-bromomethyl-4-methyl-1,3-thiazol-2(3H)-ylidene)carbamate (3.1 g) as a brown oily matter. The resulting compound and 1-(3-((6-chloro-2-naphthyl)sulfonyl)propionyl)piperazine (1.0 g) obtained in Example 3a) were dissolved in DMF (30 mL). Potassium carbonate (0.75 g) was added thereto and the mixture was mixed at 70° C. for 4 hours. The solvent was distilled off, and the residue was poured into water. The mixture was extracted with a mixed solution of chloroform-methanol, and the extract was dried over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was purified with a basic silica gel column to give the title compound (1.2 g) as a white powder.

Provenance & Evidence