反应详情

温度

80 °C

A mixture of 3.8 g of the produced 2-propyl-1,2,3,4-tetrahydronaphthalen-6-yl trifluoromethanesulfonate, 3.0 g of 3,4,5-trifluorophenylboric acid (this compound was produced by reacting a Grignard reagent prepared from 3,4,5-trifluorobromobenzene and magnesium, with trimethoxy borane, and then performing a hydrolysis with dilute hydrochloric acid), 0.13 g of tetrakis(triphenylphosphine)palladium(0), and 3.6 g of potassium phosphate in 20 ml of dimethyl formamide (DMF) was stirred for 10 hours at 80° C. The mixture was subsequently cooled to room temperature, 20 ml of water was added, the mixture was extracted with toluene, and the organic layer was washed subsequently with water and then a saturated aqueous solution of sodium chloride, and subsequently dried over anhydrous sodium sulfate. The crude product obtained by removal of the solvent by evaporation was purified by silica gel column chromatography (hexane) and then recrystallized 3 times from ethanol to obtain 0.5 g of 2-propyl-6-(3,4,5-trifluorophenyl)-1,2,3,4-tetrahydronaphthalene.

1. customwas produced
2. temperatureThe mixture was subsequently cooled to room temperature
3. extractionthe mixture was extracted with toluene
4. washthe organic layer was washed subsequently with water
5. dry with materiala saturated aqueous solution of sodium chloride, and subsequently dried over anhydrous sodium sulfate
6. customThe crude product obtained by removal of the solvent by evaporation
7. customwas purified by silica gel column chromatography (hexane)
8. customrecrystallized 3 times from ethanol