HRID1096616

反应详情

EQUATION

反应方程式

HRID 1096616 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customequipped with a reflux condenser
  2. temperaturethe solution was heated
  3. temperatureto reflux for 15 min
  4. customThe ethanol was then removed in-vacuo
  5. extractionThe resultant solution was extracted with EtOAc
  6. customThe organic layer was collected
  7. dry with materialdried with Na2SO4
  8. filtrationThis was then filtered
  9. concentrationconcentrated
  10. customdried in-vacuo