반응 #86187

반응 방정식

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

수율 65.5%

용매

dichloromethane

반응 조건

후처리

1. 1
   농축The mixture was concentrated
2. 2
   기타the residue was purified on silica
3. 3
   세척eluted with 0 to 40% EtOAc in DCM

실험 절차

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%).

출처