反应详情

温度

110 °C

4-(4-Iodo-phenyl)-piperazine-1-carboxylic acid tert-butyl ester (0.194 g, 0.5 mmol), Cul (0.01 g), Cs2CO3 (0.326 g, 1.0 mmol), [1,10]Phenanthroline (0.027 g, 0.15 mmol) and imidazole (0.034 g, 0.5 mmol) were mixed in 3 mL dry DMF in a pressure vessel. The vessel was heated at 110° C. overnight. After cooling to rt, the insoluble was filtered and washed with CH2Cl2. The filtrate was concentrated and the crude was purified with prep TLC (7.5% MeOH-2M NH3/CH2Cl2) to yield the title compound (0.077 g). M+H 328.

1. temperatureAfter cooling to rt
2. filtrationthe insoluble was filtered
3. washwashed with CH2Cl2
4. concentrationThe filtrate was concentrated
5. customthe crude was purified with prep TLC (7.5% MeOH-2M NH3/CH2Cl2)