反应详情

温度

80 °C

A mixture of 4-iodoaniline (0.654 g, 3 mmol), piperazine-1-carboxylic acid tert-butyl ester (0.67 g, 3.6 mmol), potassium phosphate (1.272 g, 6 mmol), ethylene glycol (0.33 ml) and copper iodide (0.03 g, 0.15 mmol) in 2-propanol (3 ml) was placed under argon in a sealed-tube and heated to 80° C. for 30 hours. After being cooled to room temperature, the medium was washed with water (50 ml) and extracted with ethyl acetate (100 ml). The organic layer was dried over MgSO4, concentrated and chromatographed (dichloromethane:acetone, 70:30) to yield 43a (0.36 g, 1.3 mmol, 43%) as a yellow powder.

1. customwas placed under argon in a sealed-tube
2. temperatureAfter being cooled to room temperature
3. washthe medium was washed with water (50 ml)
4. extractionextracted with ethyl acetate (100 ml)
5. dry with materialThe organic layer was dried over MgSO4
6. concentrationconcentrated
7. customchromatographed (dichloromethane:acetone, 70:30)