HRID733744

反应详情

EQUATION

反应方程式

HRID 733744 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Ethyl 4-chloro-1H-pyrrolo[3,2-c]pyridine-7-carboxylate (0.10 g) was dissolved in dimethylformamide (2 ml), cooled to 0° C. and sodium hydride (60% dispersion in oil) (0.027 g) added. The reaction mixture was stirred for 45 minutes at 0° C., allowed to warm to room temperature and stirred for a further 45 minutes. The reaction mixture was cooled to 0° C., ethyl iodide (0.039 ml) added, the reaction mixture allowed to warm to room temperature, and stirred for 1 hour. The reaction mixture was partitioned between ethyl acetate and water, the aqueous was separated and extracted three times with ethyl acetate. The combined organic layers were washed with brine, dried (MgSO4), filtered and evaporated to afford the title compound as a yellow oil (0.095 g).

WORKUP

后处理

  1. temperatureto warm to room temperature
  2. stirringstirred for a further 45 minutes
  3. temperatureThe reaction mixture was cooled to 0° C.
  4. temperatureto warm to room temperature
  5. stirringstirred for 1 hour
  6. customThe reaction mixture was partitioned between ethyl acetate and water
  7. customthe aqueous was separated
  8. extractionextracted three times with ethyl acetate
  9. washThe combined organic layers were washed with brine
  10. dry with materialdried (MgSO4)
  11. filtrationfiltered
  12. customevaporated