反应详情

In a 500 mL three-neck flask, 3.20 g of 2,3-difluoro-4-ethoxybenzoic acid (a) and 3.84 g of 2,3-difluoro-4-(trans-4-propylcyclohexyl)phenol (1) were dissolved in 230 mL of methylene chloride. 0.70 g of 4-dimethylaminopyridine was added thereto and stirred at room temperature for 1 hour. A solution in which 3.54 g of N,N-dicyclohexylcarbodiimide was dissolved in 90 mL of methylene chloride was added thereto and stirred overnight. Diethyl ether was added and urea precipitated was filtered off. Saturated aqueous solution of sodium chloride was added and stirred for 1 hour. After organic layer was separated, the organic layer was washed with 3N hydrochloric acid and saturated aqueous solution of sodium bicarbonate, and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to give 6.60 g of 2,3-difluoro-4-(trans-4-propylcyclohexyl)phenyl 4-ethoxy-2,3-difluorobenzoate (m).

1. additionwas added
2. stirringstirred overnight
3. customurea precipitated
4. filtrationwas filtered off
5. additionSaturated aqueous solution of sodium chloride was added
6. stirringstirred for 1 hour
7. customAfter organic layer was separated
8. washthe organic layer was washed with 3N hydrochloric acid and saturated aqueous solution of sodium bicarbonate
9. dry with materialdried over anhydrous sodium sulfate
10. distillationThe solvent was distilled off under reduced pressure