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
The synthesis was performed with reference to the known literature (US 2006/0148801). A solution of 6-methyl-1-tosyl-1H-pyrrolo[2,3-b]pyridine (0.17 g, 0.60 mmol) in ethanol (5.0 mL) was added with 5 N aqueous sodium hydroxide (1.0 mL), and the mixture was refluxed for 8 hours by heating. The solvent was evaporated under reduced pressure, the residue was extracted with chloroform, and then the organic layer was washed successively with water and saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and then the residue was subjected to silica gel column chromatography (eluted with hexane/ethyl acetate (80:20→60:40)) to obtain 6-methyl-1H-pyrrolo[2,3-b]pyridine (0.071 g, 90%).
WORKUP
后处理
- temperaturethe mixture was refluxed for 8 hours
- temperatureby heating
- customThe solvent was evaporated under reduced pressure
- extractionthe residue was extracted with chloroform
- washthe organic layer was washed successively with water and saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- customThe solvent was evaporated under reduced pressure
- washthe residue was subjected to silica gel column chromatography (eluted with hexane/ethyl acetate (80:20→60:40))