反应详情

温度

65 °C

Into a solution of 5-bromo-2-nitropyridine (30 g, 148 mmol) in DMSO (350 mL) were added K2CO3 (14 g, 104 mmol) and (3S)-tert-butyl-3-methylpiperazine-1-carboxylate (10.0 g, 50 mmol). The mixture was stirred at 65° C. overnight and then after cooling to room temperature, poured into water (700 mL). The solid precipitate was collected and dried under vacuum. It was further purified on a flash column eluting with 20:1 petroleum ether/ethyl acetate and then with CH2Cl2 to give 105a as a yellow solid (8.05 g, 50%). LCMS: [M+H]+ 323

1. temperatureafter cooling to room temperature
2. customThe solid precipitate was collected
3. customdried under vacuum
4. customIt was further purified on a flash column
5. washeluting with 20:1 petroleum ether/ethyl acetate