反应详情

In a solution of 0.23 g of N-(6-bromo-2-pyridyl)-4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydro-isoxazole-3-yl]-2-methyl benzoic acid amide in 5 mL of N,N-dimethylformamide, 0.02 g of 55% oily sodium hydride was added at room temperature with stirring, and stirred at the same temperature for 10 minutes. After ceasing the generation of hydrogen gas, 0.30 g of methyl iodide was added, and continued to stir further for 45 minutes. After the completion of the reaction, the reaction mixture was poured in 20 mL of ice water, extracted with ethyl acetate (50 mL×1), the organic phase was dehydrated with and dried over saturated sodium chloride aqueous solution and then anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified with silica gel column chromatography that was eluated with ethyl acetate-hexane (1:2) to obtain 0.18 g of the aimed product as colorless resinous substance.

1. stirringstirred at the same temperature for 10 minutes
2. additionwas added
3. stirringto stir further for 45 minutes
4. customAfter the completion of the reaction
5. extractionextracted with ethyl acetate (50 mL×1)
6. dry with materialdried over saturated sodium chloride aqueous solution
7. distillationanhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure
8. customThe residue was purified with silica gel column chromatography that