反应详情

To a rt solution of 550 mg of 3-methyl-5-phenyl-1H-pyrazol-4-ylamine (prepared in accordance with the procedure set forth in UK 2 185 255, Example 2A) in 8.5 mL pyridine was added 370 μL of benzoyl chloride. The reaction was stirred for 1 h and then concentrated under reduced pressure. The residue was dissolved in chloroform and washed with 0.5 N hydrochloric acid and then saturated aqueous sodium carbonate. The organic portion was dried with sodium sulfate and concentrated under reduced pressure and purified by means of MPLC (12 g SiO2, 40% ethyl acetate:heptane) to give the title compound as a colorless solid.

1. concentrationconcentrated under reduced pressure
2. dissolutionThe residue was dissolved in chloroform
3. washwashed with 0.5 N hydrochloric acid
4. dry with materialThe organic portion was dried with sodium sulfate
5. concentrationconcentrated under reduced pressure
6. custompurified by means of MPLC (12 g SiO2, 40% ethyl acetate:heptane)