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General procedure: A 25 mL Schlenk tube wascharged with a magnetic stirrer and DMSO (2.0 mL). Substituted(2-bromophenyl)methylamine (1) (0.5 mmol), amidine hydrochloride (2) (1.0 mmol),CuBr (0.1 mmol, 14.2 mg), and K2CO3 (1.5 mmol, 207 mg) were added to the tube.The mixture was stirred at 80-120 oC under nitrogen atmosphere for 24 h, and thenunder air for 0.5 h. The resulting mixture was cooled to room temperature and filtered,and the solid was washed with ethyl acetate for two times (3 × 3 mL). The combinedfiltrate was concentrated by the rotary evaporator, and the residue was purified bycolumn chromatography on silica gel using petroleum ether/ ethyl acetate as eluent togive the desired target product.
With potassium phosphate; copper(l) iodide; Trimethylacetic acid; In 1,2-dichloro-benzene; at 110℃; for 18h;Sealed tube;
General procedure: Anoven-dried 10mLvialwas charged with CuI (9mg, 0.05mmol),K3PO4 (318 mg, 1.5 mmol), pivalic acid (20 mg, 0.2 mmol), a 1-(2-bromophenyl)methanamine 1 (0.5 mmol), and an amidinium salt 2or an imidate salt 4 (0.5 mmol) under air. After sealing the vial, dry1,2-dichlorobenzene (3 mL) was added by syringe and the reactionmixture was stirred at 110 C (oil bath temperature) for 18 h. Aftercooling to room temperature, the vial was opened and the reactionmixturewas partitioned between CH2Cl2 (30 mL) and brine (20 mL).The aqueous phase was extracted with CH2Cl2 (220 mL). Thecombined organic layers were dried over anhydrous MgSO4 andconcentrated in vacuum. The residue was purified by flash chromatographyon silica gel to afford the desired product.
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