反应详情

温度

120 °C

Charge in a pressure tube copper iodide (16 mg, 0.08 mmol), potassium phosphate (717 g, 3.4 mmol), trans-1,2-diaminocyclohexane (0.020 ml, 0.17 mmol), 1-Iodo-2-(3-methyl-butyl)-benzene (462 mg, 1.7 mmol) and 3-oxo-piperazine-1-carboxylic acid tert-butyl ester (405 g, 2.02 mmol). Purge with nitrogen and add 2 ml of dry 1,4-dioxane. Cap the tube and stir at 120° C. overnight. Filter through celite eluting with EtOAc and concentrate. Purify in a silica gel cartridge (10 g) eluting with hexane followed by EtOAc/hexane 1:1 to give the title compound as a yellow solid (172 mg, 29%).

1. customPurge with nitrogen
2. additionadd 2 ml of dry 1,4-dioxane
3. customCap the tube
4. filtrationFilter through celite
5. washeluting with EtOAc
6. concentrationconcentrate
7. customPurify in a silica gel cartridge (10 g)
8. washeluting with hexane