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4-bromo-2-fluoro-4'-(trans-4-pentylcyclohexyl)biphenyl[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
67.8%
With sodium carbonate;tetrakis(triphenylphosphine) palladium(0); In ethanol; water; benzene; for 37h;Heating / reflux;
First, 150 ml of ethanol containing 17.84 g of <strong>[143651-26-7]4-(trans-4-pentylcyclohexyl)phenylboronic acid</strong> dissolved therein, 150 ml of benzene containing 15.0 g of 4-bromo-2-fluoro-1-iodobenzene dissolved therein, 49.8 ml of a sodium carbonate aqueous solution with a concentration of 2.0 mol/l, and 1.44 g of tetrakis(triphenylphosphine)palladium(0) were put in an argon-replaced 500 ml flask, and stirred under reflux for 37 hours. After the reaction, water and ether were added to the reaction solution for extraction. The resultant ether layer was washed with a saturated brine and dried with sodium sulfate. The solvent was then distilled off. The residue was purified by silica gel column chromatography (eluent:hexane) and recrystallized from hexane, to obtain 13.6 g (Y: 67.8%) of 4-bromo-2-fluoro-4'-(trans-4-pentylcyclohexyl)biphenyl. The purity of the resultant compound was 99.5% as measured by GC.
tert-butyl 3-(4-bromo-2-fluorophenyl)-5,6-dihydropyridine-1(2H)carboxylate[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
75%
With (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; In 1,4-dioxane; water; at 70℃; for 3h;Inert atmosphere;
mixture of tert-butyl 3 -(4,4,5,5-tetramethyl- 1,3 ,2-dioxaborolan-2-yl)-5,6-dihydropyridine- 1 (2H)-carboxylate (4.3 g, 13.9 mmol), 4-bromo-2-fluoro- 1 -iodobenzene (6.2520.8 mmol), [1,1 ?-Bis(diphenylphosphino)ferrocene] dichloropalladium(II) (2.54 g, 2.78 mmol) and potassium carbonate (5.75 g, 41.7 mmol) in dioxane/H20 (L/10 mL) was degassed withNitrogen for three times and then heated at 70 °C for 3 h. The reaction mixture was cooled to room temperature and concentrated to get crude product, which was purified by silica gel chromatography (petroleum ether/ethyl acetate = 4/1) to afford the title compound (3.7 g, yield 75percent) as a brown oil. MS (ES+) C16H19BrFNO2 requires: 355, found: 300 [M-56+H].
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