反应详情

温度

220 °C

A mixture of 2,3-dichloropyrazine (4.9 g, 32.9 mmol), 1-benzyl-cis-3,5-dimethylpiperazine (5.9 g, 29.0 mmol), tributylamine (5.9 g, 32 mmol) and diphenyl ether (70 mL) was heated in a sealed tube at 220° C. for 3 days. The reaction mixture was cooled to ambient temperature and EtOAc (200 mL) and toluene (100 mL) were added. The organic phase was extracted with 5 M aqueous HCl (×3) and the combined aqueous phases were extracted with CHCl3 (×3). The combined organic layers, which contained the product, were washed with aqueous NaOH (5 M), dried (MgSO4), and the solvent was evaporated. The crude product (0.96 g), about 80% pure based on GC, was used in the next step without further purification.

1. temperatureThe reaction mixture was cooled to ambient temperature
2. extractionThe organic phase was extracted with 5 M aqueous HCl (×3)
3. extractionthe combined aqueous phases were extracted with CHCl3 (×3)
4. washwere washed with aqueous NaOH (5 M)
5. dry with materialdried (MgSO4)
6. customthe solvent was evaporated
7. customwas used in the next step without further purification