HRID2373207
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperatureAfter cooling
- customthe residue was evaporated
- additionThe residue was diluted with CHCl3
- washwashed with saturated NaHCO3, water
- dry with materialdried over anhydrous MgSO4
- concentrationconcentrated in vacuo
- customThe residue was purified by flash column chromatography on silica gel eluting with a mixture of EtOAc and n-hexane (1:7)-to