反应详情

70 ml of 1.69M n-hexane solution of n-butyllithium was added dropwise to solution of 18 ml of diisopropylamine in 75 ml of tetrahydrofuran at −65 ° C. under nitrogen stream, and the mixture was stirred at the same temperature for 15 minutes. To the solution was added dropwise solution of 9.5 g of 2,4,5-trifluoro-3-methylbenzoic acid in 75 ml of tetrahydrofuran at −60° C., and the mixture was stirred at the same temperature for 15 minutes. To the solution was added dropwise 9.5 ml of methyl iodide at −70° C., and the mixture was stirred at the same temperature for 30 minutes and overnight at room temperature. Diethylether and water were added for separation, and the aqueous layer was collected. The aqueous layer was acidified by adding conc. hydrochloric acid, and extracted with diethylether. The organic layer was dried over ahnydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain 6.6 g of the title compound.

1. stirringthe mixture was stirred at the same temperature for 15 minutes
2. stirringthe mixture was stirred at the same temperature for 30 minutes and overnight at room temperature
3. customthe aqueous layer was collected
4. additionby adding conc. hydrochloric acid
5. extractionextracted with diethylether
6. dry with materialThe organic layer was dried over ahnydrous magnesium sulfate
7. distillationthe solvent was distilled off under reduced pressure