反应详情

温度

0 °C

Step 4): LiAlH4 (0.14 g, 3.7 mmol) was added to a solution of 11-(4-hydroxyiminopiperidin-1-yl)-2-bromo-6,11-dihydrodibenz[b,e]oxepin (1.5 g, 3.7 mmol) in dry THF (50 ml) under nitrogen atmosphere. The reaction mixture was heated at 60°-70° C. for 3 hours. After cooled at 0° C., the reaction mixture was hydrolyzed with water and diluted with ether, then filtered. The filtrate was concentrated to give 11-(4-aminopiperidin-1-yl)-2-bromo-6,11-dihydrodibenz[b,e]oxepin (69.1%): mp 142°-144° C.

1. temperatureThe reaction mixture was heated at 60°-70° C. for 3 hours
2. filtrationfiltered
3. concentrationThe filtrate was concentrated