HRID2373207

反应详情

EQUATION

反应方程式

HRID 2373207 的结构方程式

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A mixture of 5-amino-1-ethylpyrazole (250 mg) and ethyl 2-acetyl-3-(3-chlorophenyl)acrylate (568 mg) was heated at 130° C. for 3 hours. After cooling, the residue was evaporated. The residue was diluted with CHCl3 and washed with saturated NaHCO3, water, dried over anhydrous MgSO4 and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel eluting with a mixture of EtOAc and n-hexane (1:7)-to give ethyl 4-(3-chlorophenyl)-1-ethyl-6-methyl-4,7-dihydro-1H-pyrazolo[3,4-b]pyridine-5-carboxylate (271 mg) as a yellow oil.

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe residue was evaporated
  3. additionThe residue was diluted with CHCl3
  4. washwashed with saturated NaHCO3, water
  5. dry with materialdried over anhydrous MgSO4
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified by flash column chromatography on silica gel eluting with a mixture of EtOAc and n-hexane (1:7)-to