HRID1501571
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a stirred solution of ethyl 6-bromo-1H-pyrazolo[3,4-b]pyridine-4-carboxylate (20 g, 74.3 mmol) in acetonitrile (200 mL), K2CO3 (15.39 g, 111.52 mmol) and 2-bromopropane (18.13 g, 148.64 mmol) was added to it. The reaction mixture was refluxed for 8 h. On completion, acetonitrile was removed under reduced pressure and water was added to it. Extraction was carried out using ethyl acetate; the combined organic layers were washed with water, brine and dried over anhydrous Na2SO4. Solvent was removed under reduced pressure and residue was purified by silica gel column chromatography to obtain the desired intermediate (13.5 g, 58.3%).
WORKUP
后处理
- temperatureThe reaction mixture was refluxed for 8 h
- customOn completion, acetonitrile was removed under reduced pressure and water
- additionwas added to it
- extractionExtraction
- washthe combined organic layers were washed with water, brine
- dry with materialdried over anhydrous Na2SO4
- customSolvent was removed under reduced pressure and residue
- customwas purified by silica gel column chromatography