HRID2253385

反应详情

EQUATION

反应方程式

HRID 2253385 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A suspension of 7-[2,6-dimethoxy-4-(methoxymethyl)phenyl]-2-ethyl-3-nitropyrazolo[1,5-a]pyridine (0.7 g) in a mixed solvent of ethanol (35 mL), water (18 mL) and acetic acid (3.5 mL) was added zinc powder (0.7 g) at room temperature, and the reaction mixture was heated and stirred for 30 minutes at 60° C. The reaction mixture was filtered through celite to remove insoluble residue, water was added to the filtrate and extraction was performed with ethyl acetate. The obtained organic extract was washed with brine, saturated aqueous sodium bicarbonate and then brine and dried over anhydrous magnesium sulfate and filtered, after which the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography and the title compound (0.48 g) was obtained as a yellow oil from the n-hexane:ethyl acetate (4:1) fraction.

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. filtrationThe reaction mixture was filtered through celite
  3. customto remove insoluble residue, water
  4. additionwas added to the filtrate and extraction
  5. extractionThe obtained organic extract
  6. washwas washed with brine, saturated aqueous sodium bicarbonate
  7. dry with materialbrine and dried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. customafter which the solvent was evaporated under reduced pressure
  10. customThe residue was purified by silica gel column chromatography