HRID350019

反应详情

EQUATION

反应方程式

HRID 350019 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of ethyl 1-benzyl-3-ethoxy-1H-pyrazol-4-ylacetate (7.50 g), 5% palladium-carbon (15.0 g), formic acid (50 ml) and ethanol (100 ml) was refluxed for 1 hour. After cooling, the palladium-carbon was removed by filtration, and the filtrate was concentrated. The residue was dissolved in ethyl acetate, which was washed with saturated aqueous sodium bicarbonate solution, and with a saturated aqueous sodium chloride solution, dried (MgSO4) and concentrated. The residue was subjected to silica gel column chromatography to obtain ethyl 3-ethoxy-1H-pyrazol-4-ylacetate (2.79 g, yield 54%) as a colorless oily substance from the fraction eluted with ethyl acetate-hexane (1:1, volume ratio).

WORKUP

后处理

  1. temperaturewas refluxed for 1 hour
  2. temperatureAfter cooling
  3. customthe palladium-carbon was removed by filtration
  4. concentrationthe filtrate was concentrated
  5. dissolutionThe residue was dissolved in ethyl acetate
  6. washwhich was washed with saturated aqueous sodium bicarbonate solution
  7. dry with materialwith a saturated aqueous sodium chloride solution, dried (MgSO4)
  8. concentrationconcentrated