反应详情

温度

60 °C

To a mixture of 3-bromo-5-(2-chloro-4-fluorophenyl)-1-methyl-1H-pyrazole (i.e. the product of Step C) (620 mg, 2.14 mmol) in N,N-dimethylformamide (8 mL) at 60° C. was added N-iodosuccinimide (963 mg, 4.28 mmol). The reaction mixture was stirred at 60° C. for 3 h, and then diluted with ethyl acetate, washed with water and saturated aqueous sodium chloride solution, dried over sodium sulfate and concentrated under reduced pressure. The material was purified by silica gel chromatography (5 to 30% gradient of ethyl acetate in hexanes as eluant) to provide the title compound as a pale yellow solid (515 mg) melting at 139-141° C.

1. washwashed with water and saturated aqueous sodium chloride solution
2. dry with materialdried over sodium sulfate
3. concentrationconcentrated under reduced pressure
4. customThe material was purified by silica gel chromatography (5 to 30% gradient of ethyl acetate in hexanes as eluant)