反应详情

In a solution of 0.25 g of 4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole-3-yl]-2-methyl-N-(5-pyrimidinyl)benzoic acid amide in 4 mL of N,N-dimethylformamide, 0.36 g of methyl iodide and 0.35 g of potassium carbonate were added at room temperature with stirring, and stirred at 80° C. for 1 hour. After the completion of the reaction, 10 mL of water was added in the reaction mixture, and extracted with ethyl acetate (20 mL×1), the organic phase was dehydrated with and dried over saturated sodium chloride aqueous solution and then anhydrous sodium 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 0.09 g of the aimed product as white crystal.

1. stirringstirred at 80° C. for 1 hour
2. additionwas added in the reaction mixture
3. extractionextracted with ethyl acetate (20 mL×1)
4. dry with materialdried over saturated sodium chloride aqueous solution
5. distillationanhydrous sodium sulfate, and the solvent was distilled off under reduced pressure
6. customThe residue was purified with silica gel column chromatography that