HRID1864997

反应详情

EQUATION

反应方程式

HRID 1864997 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

After dissolving 7-bromo-2-methoxypyrazolo[1,5-a]pyridine (1 g) in acetic acid (10 mL), an aqueous solution (5 mL) containing sodium nitrite (334 mg) was added and the mixture was stirred at room temperature for 20 minutes. After adding ethanol (60 mL) and water (30 mL) to the reaction mixture, zinc powder (1 g) was added and the mixture was heated and stirred at 60° C. for 30 minutes. The insoluble residue was filtered out, water was added, and extraction was performed with ethyl acetate. After washing the organic layer with brine, drying it over anhydrous magnesium sulfate and filtering it, the solvent was concentrated under reduced pressure, the residue was purified by silica gel column chromatography, and the title compound (750 mg) was obtained from the n-hexane:ethyl acetate (3:1) fraction as brown crystals.

WORKUP

后处理

  1. additionwas added
  2. additionwas added
  3. temperaturethe mixture was heated
  4. stirringstirred at 60° C. for 30 minutes
  5. filtrationThe insoluble residue was filtered out
  6. additionwater was added
  7. extractionextraction
  8. washAfter washing the organic layer with brine
  9. dry with materialdrying it over anhydrous magnesium sulfate
  10. filtrationfiltering it
  11. concentrationthe solvent was concentrated under reduced pressure
  12. customthe residue was purified by silica gel column chromatography