反应详情

580 mg of 4-bromo-3-methylpyrazole, 1.0 g of 2-fluorophenylboric acid, 3.3 g of copper acetate, 1.0 g of molecular sieves 4A, and 1.6 ml of pyridine were suspended in 8.0 ml of dimethylformamide, and the mixture was stirred at room temperature for 3 days. The obtained suspended solution was filtrated by celite, and the filtrate was diluted with ethyl acetate. Organic layer was washed with 0.5 N sodium hydride, dried with sodium sulfate, and the solvents were distilled outunder reduced pressure. The residues were purified by silicagel column chromatography (hexane:ethyl acetate=50:50) to obtain 78 mg of the above compound as a crude product.

1. filtrationwas filtrated by celite
2. additionthe filtrate was diluted with ethyl acetate
3. washOrganic layer was washed with 0.5 N sodium hydride
4. dry with materialdried with sodium sulfate
5. distillationthe solvents were distilled outunder reduced pressure
6. customThe residues were purified by silicagel column chromatography (hexane:ethyl acetate=50:50)