反应详情

温度

100 °C

A mixture of D10 (1.083 g, 3.955 mmol), 2,2-dimethyl-1-phenylpiperazine (0.903 g, 4.745 mmol) [C.A.S. 2946-75-0] and DIPEA (1.378 ml, 7.909 mmol) in CH3CN (15 ml) was heated in a sealed tube at 100° C. for 5 days. After cooling, the solvent was concentrated in vacuo. The residue was purified by column chromatography (silica gel; Heptane/EtOAc 100/10 to 80/20 as eluent). The desired fractions were collected and concentrated in vacuo to yield intermediate D55 (0.56 g, 42%).

1. temperatureAfter cooling
2. concentrationthe solvent was concentrated in vacuo
3. customThe residue was purified by column chromatography (silica gel; Heptane/EtOAc 100/10 to 80/20 as eluent)
4. customThe desired fractions were collected
5. concentrationconcentrated in vacuo
6. customto yield intermediate D55 (0.56 g, 42%)