反応 #86187

反応方程式

1-(6-bromo-3-methoxy-2-pyridyl)-1,4-diazepan-6-ol

tert-butoxycarbonyl tert-butyl carbonate

sodium bicarbonate

→

tert-butyl 4-(6-bromo-3-methoxy-2-pyridyl)-6-hydroxy-1,4-diazepane-1-carboxylate

収率 65.5%

溶媒

dichloromethane

反応条件

後処理

1. 1
   濃縮The mixture was concentrated
2. 2
   その他the residue was purified on silica
3. 3
   洗浄eluted with 0 to 40% EtOAc in DCM

実験手順

A mixture of 1-(6-bromo-3-methoxy-2-pyridyl)-1,4-diazepan-6-ol (0.9968 mmol; 301.2 mg), tert-butoxycarbonyl tert-butyl carbonate (1.495 mmol; 326.3 mg), and sodium bicarbonate (9.968 mmol; 837.4 mg) in dichloromethane (20 Ml) was stirred at room temperature overnight. The mixture was concentrated, and the residue was purified on silica eluted with 0 to 40% EtOAc in DCM to afford tert-butyl 4-(6-bromo-3-methoxy-2-pyridyl)-6-hydroxy-1,4-diazepane-1-carboxylate (262.5 mg, 65%).

出典