三氟乙酰三氟甲磺酸酯

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To 50 ml of carbon tetrachloride were added 3.9 g (18 mmol) of 4-(4-propylcyclohexyl)cyclohexanone and 3.8 g (19 mmol) of 2,6-di-t-butyl-4-methylpyridine, and the mixture was stirred at room temperature. To this mixture was added dropwise 2 ml of solution of 4.5 g (18 mmol) of trifluoroacetyltriflate in carbon tetrachloride. Subsequently, 25 ml of carbon tetrachloride was added thereto and the mixture was stirred at room temperature for 1 hour. The reaction solution was filtered off and then the filtrate was concentrated under a reduced pressure. After the residue was purified by column chromatography on silica gel (eluent: heptane/toluene=3/1), the solvent was distilled off, and the residue was subjected twice to recrystallization by using heptane to give 1.3 g (4.1 mmol) of trifluoroacetic acid 4-(4-propylcyclohexyl)-1-cyclohexenyl ester. Yield of this compound based on 4-(4-propylcyclohexyl)cyclohexanone was 23%. the mixture was stirred at room temperature for 1 hour The reaction solution was filtered off the filtrate was concentrated under a reduced pressure After the residue was purified by column chromatography on silica gel (eluent: heptane/toluene=3/1) the solvent was distilled off the residue was subjected twice to recrystallization