反应详情

温度

110 °C

To 0.200 g (0.689 mmole) of ethyl 7-fluoro-2-(trifluoromethyl)-2H-chromene-3-carboxylate in 2.5 mL of DMF was added 0.118 g (0.946 mmol) of 2,5-dimethyl phenol to the vessel followed by 0.131 g (0.946 mmole) of potassium carbonate. The suspension was prepared in a capped vial and placed in a J-KEM heating block equipped with shaker, condenser and nitrogen atmosphere. The block was heated to 110° C. for 20hrs. For work up, 10 mL of H2O and 5 mL of ether was added to the mixture. The organic layer was separated and then the aqueous was extracted 3 times with ether. The product was then run through a pre-packed silica gel plug (20 mL, 5 g capacity) and the silica column washed with 4×5 mL aliquots of ether. Concentration of the solution afforded the product with was used directly in the next step without further purification.

1. customThe suspension was prepared in a capped vial and
2. customequipped with shaker, condenser and nitrogen atmosphere
3. customThe organic layer was separated
4. extractionthe aqueous was extracted 3 times with ether
5. washthe silica column washed with 4×5 mL aliquots of ether
6. customConcentration of the solution afforded the product
7. customwith was used directly in the next step without further purification