HRID452523

反应详情

EQUATION

反应方程式

HRID 452523 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a solution of 1.25 g of N-[4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazol-3-yl]-2-methyl benzoic acid amide synthesized in Synthetic Example 29 and 0.32 g of 2,3-dihydrofuran in 30 ml of dichloromethane, 0.01 g of p-toluene sulfonic acid monohydrate was added with stirring at room temperature, and stirred at room temperature for 3 days. After the completion of the reaction, 30 ml of saturated sodium hydrogen carbonate aqueous solution was added in the reaction mixture, and extracted with ethyl acetate (30 ml×2), the organic phase was dehydrated and dried with saturated sodium chloride aqueous solution and anhydrous sodium sulfate in that order, and the solvent was distilled under reduced pressure. The residue was purified with silica gel column chromatography that was eluated with ethyl acetate-hexane (1:1) to obtain 1.18 g of the aimed product as colorless resinous substance.

WORKUP

后处理

  1. additionwas added
  2. stirringstirred at room temperature for 3 days
  3. additionwas added in the reaction mixture
  4. extractionextracted with ethyl acetate (30 ml×2)
  5. dry with materialdried with saturated sodium chloride aqueous solution and anhydrous sodium sulfate in that order
  6. distillationthe solvent was distilled under reduced pressure
  7. customThe residue was purified with silica gel column chromatography that