反应详情

温度

130 °C

0.54 g of 3-trifluoromethylheptyl p-toluenesulfonate obtained in Step 1), 0.27 g of ethyl p-hydroxybenzoate and 1 ml of dimethylformamide (DMF) were placed in a round-bottomed flask, and 0.07 g of sodium 60%-hydride was added thereto together with DMF, followed by 6 hours of stirring at 130° C. After the reaction, DMF was distilled off under a reduced pressure, and water was added, followed by extraction with diethyl ether. The ether solution was dried with sodium sulfate, followed by distilling-off of the solvent to obtain 0.62 g of a crude product. The crude product was then purified by thin layer chromatography with benzene as the developer to obtain 0.22 g of ethyl p-(3-trifluoromethylheptyloxy)benzoate (yield: 42%).

1. distillationwas distilled off under a reduced pressure, and water
2. additionwas added
3. extractionfollowed by extraction with diethyl ether
4. dry with materialThe ether solution was dried with sodium sulfate
5. customto obtain 0.62 g of a crude product
6. customThe crude product was then purified by thin layer chromatography with benzene as the developer