反应详情

In a round-bottomed flask, 0.88 g of the 3-trifluoromethylheptyl p-toluenesulfonate 2, 0.4 g of ethyl p-hydroxybenzoate and 1 ml of dimethylformamide were placed, and 50 mg of sodium hydride was added thereto, followed by 8 hours of heat-refluxing and 15 hours of standing at room temperature. After the reaction, dimethylformamide was distilled off, and dilute hydrochloric acid was added to the product, which was then extracted with methylene chloride. The resultant organic layer was washed with water and dried with magnesium sulfate, followed by distilling-off of the solvent and purification by thin layer chromatography (developer: methylene chloride/ hexane=1/1) to obtain 0.7 g of ethyl p-(3-trifluoromethylheptyloxy)benzoate 3. (Yield: 80%)

1. temperatureof heat-refluxing and 15 hours
2. customof standing at room temperature
3. distillationwas distilled off
4. additiondilute hydrochloric acid was added to the product, which
5. extractionwas then extracted with methylene chloride
6. washThe resultant organic layer was washed with water
7. dry with materialdried with magnesium sulfate
8. distillationfollowed by distilling-off of the solvent and purification by thin layer chromatography (developer: methylene chloride/ hexane=1/1)