反应详情

温度

100 °C

A mixture of 2-bromo-6-fluoropyridine (500 mg, 2.8 mmol), tert-butyl 1,4-diazepane-1-carboxylate (568 mg, 2.8 mmol) in DIPEA (1.83 g, 14.2 mmol) and ethanol (10 mL) was heated at 100° C. for 16 hours. After it was cooled, the solvent was removed under reduced pressure, and the residue was diluted with EtOAc (100 mL) and washed with brine. The organic layer was dried over Na2SO4 and concentrated under reduced pressure to afford tert-butyl 4-(6-bromopyridin-2-yl)-1,4-diazepane-1-carboxylate as a colorless oil (500 mg, 50%). MS (ESI) m/z: 356 [M+H]+.

1. temperatureAfter it was cooled
2. customthe solvent was removed under reduced pressure
3. additionthe residue was diluted with EtOAc (100 mL)
4. washwashed with brine
5. dry with materialThe organic layer was dried over Na2SO4
6. concentrationconcentrated under reduced pressure