反应详情

To a solution of 5-((4-bromo-2-chlorophenyl)amino)-4-fluorobenzo[d]thiazole-6-carboxylic acid (120 mg, 0.299 mmol) in t-BuOH (10 mL) was added DPPA (48 mg, 0.449 mmol) followed by triethylamine (60 mg, 0.598 mmol). The mixture was heated under reflux for 3 h and allowed to slowly warm to room temperature. The solvent was removed in vacuo and the resultant crude product was purified by column chromatography on silica gel (petroleum ether/ethyl acetate, 2:1, v/v). The corresponding product was obtained (white solid, 100 mg, 83.9% yield). 1H NMR (400 MHz, DMSO-d6): δ 11.76 (s, 1H), 8.65 (s, 1H), 7.95 (d, 1H), 7.77 (d, 1H), 7.50 (m, 1H), 7.39 (s, 1H).

1. temperatureThe mixture was heated
2. temperatureunder reflux for 3 h
3. customThe solvent was removed in vacuo
4. customthe resultant crude product was purified by column chromatography on silica gel (petroleum ether/ethyl acetate, 2:1
5. customThe corresponding product was obtained (white solid, 100 mg, 83.9% yield)