2-Naphthalenol, 1,7,8-trifluoro-

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

实验步骤: An acetone (80 ml) solution of 1,7,8-trifluoro-2-naphthol (15 g), potassium carbonate (16 g), and ethyl iodide (26 g) was stirred for 10 hours at room temperature. Toluene (200 ml) was added in this reaction solution. The organic layer was removed, and the aqueous layer was extracted with toluene. The organic layers were combined, washed with brine, and concentrated. The residue was evaporated under reduced pressure, and 2-ethoxy-1,7,8-trifluoronaphthalene was obtained. The organic layer was removed the aqueous layer was extracted with toluene washed with brine concentrated The residue was evaporated under reduced pressure

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

实验步骤: Pyridine (10 ml) was added slowly and dropwise to a dichloromethane (60 ml) solution of 1,7,8-trifluoro-2-naphthol (10 g) and trifluoromethanesulfonic acid anhydrate (10.3 ml) at the temperature of the ice/water, and then the reaction solution was stirred for 30 minutes. Water and dichloromethane were added slowly in the reaction solution. The organic layer was removed, and the aqueous layer was extracted with dichloromethane. The organic layers were combined, washed with water, 10% hydrochloric acid, a saturated sodium hydroxide aqueous solution, water, and brine consecutively, and concentrated. The residue was purified by column chromatography (silica gel, hexane/ethyl acetate=19/1), and 1,7,8-trifluoronaphthalene-2-yl trifluoromethanesulfonate was obtained as light yellow crystals. The organic layer was removed the aqueous layer was extracted with dichloromethane washed with water, 10% hydrochloric acid a saturated sodium hydroxide aqueous solution, water, and brine consecutively, and concentrated The residue was purified by column chromatography (silica gel, hexane/ethyl acetate=19/1)