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With potassium carbonate;copper(l) iodide; cis-N,N'-dimethyl-1,2-diaminocyclohexane; In N,N-dimethyl-formamide; at 130℃; for 1h;microwave irradiation;
A solution of L-1 (1.0 g, 8.4 mmol), Cul (960 mg, 5.4 mmol), K2CO3 (2.78 g, 20.2 mmol), N,N'-dimethyl-l,2-diaminocyclohexane (0.130 mL, 0.84 mmol), and L-2 (2.8 g, 11 mmol) in 13 mL of DMF is warmed at 130C in a microwave reactor. After 1 hour, the reaction is diluted with saturated aqueous NH4C1 (50 mL) and NaHCO3 is added and the mixture is stirred for 30 minutes. EtOAc (200 mL) is added and the mixture is stirred overnight at room temperature. The mixture is extracted with EtOAc (3 x 50 mL). The combined organic layers are washed with saturated aqueous NH4CI (3 x 40 mL), dried over magnesium sulfate, filtered and concentrated. The residue is dissolved in 15 mL methanol and stirred at 80C for 30 minutes and allowed to cool for 1 hour. The material is collected by filtration, washed with hexanes, and dried to provide L-3.
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