反应详情

To 50 ml of DMF were added 5.0 g of 3,4,5-trifluorobenzoic acid, 4.0 g of propargyl bromide and 4.7 g of potassium carbonate. The mixture was stirred at room temperature for 30 minutes, and then at 80° C. for 1 hour. Thereafter, ethyl acetate was added to the reaction mixture which had been allowed to cool to near room temperature, and this was filtered through Celite (registered trade mark). To the filtrate were added successively water and dilute hydrochloric acid, followed by extraction with ethyl acetate. The organic layer was dried over magnesium sulfate, and concentrated under reduced pressure, and 6.0 g of 2-propynyl 3,4,5-trifluorobenzoate was obtained.

1. waitat 80° C. for 1 hour
2. temperatureto cool to near room temperature
3. filtrationthis was filtered through Celite (registered trade mark)
4. additionTo the filtrate were added successively water and dilute hydrochloric acid
5. extractionfollowed by extraction with ethyl acetate
6. dry with materialThe organic layer was dried over magnesium sulfate
7. concentrationconcentrated under reduced pressure