反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
tert-Butyl 3-(5-methoxy-3-(3-methoxypropyl)-3H-imidazo[4, 5-13]pyridin-2-yl)piperidine-1-carboxylate (33C) (1.19 mmol; 0.481 g) was added to a 100 mL round-bottomed flask equipped with a reflux condenser and stirring under nitrogen. EtOH (15 mL) and HCl (8M in H2O; 4 mL) were then added and the solution was heated to reflux for 15 min. Analysis of the reaction mixture by LC/MS indicated that the reaction was complete at this time. The ethanol was then removed in-vacuo. The resultant solution was extracted with EtOAc and a 10% aqueous K2CO3 solution. The organic layer was collected and dried with Na2SO4. This was then filtered and concentrated and dried in-vacuo affording 5-Methoxy-3-(3-methoxypropyl)-2-(piperidin-3-yl)-3H-imidazo[4,5-b]pyridine (330) as a brown oil. (1.15 mmol, 0.351 g, 97% yield). ESI-MS: m/z 305.1 (M+H)+.
WORKUP
后处理
- customequipped with a reflux condenser
- temperaturethe solution was heated
- temperatureto reflux for 15 min
- customThe ethanol was then removed in-vacuo
- extractionThe resultant solution was extracted with EtOAc
- customThe organic layer was collected
- dry with materialdried with Na2SO4
- filtrationThis was then filtered
- concentrationconcentrated
- customdried in-vacuo