HRID40630
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
6-Methyl-pyridin-3-ol (0.218 g, 2.0 mmol) was placed in a flask with DMF (10 mL) and NaH (60% dispersion in oil, 77 mg, 2.0 mmol) and stirred for 30 min. at room temperature. (S)-glycidyl 3-nitrobenzene sulfonate (0.52 g, 2.0 mmol) was then added to the reaction mixture, which was then stirred at room temperature for 14 hours. The reaction was quenched with NaHCO3 (saturated) and then extracted three times with ethyl acetate. The organic layer was dried with magnesium sulfate, filtered and the solvent was evaporated under reduced pressure to yield crude product which was purified by silica gel chromatography (60% Ethyl acetate/heptane) to yield the title compound as a residue.
WORKUP
后处理
- stirringwas then stirred at room temperature for 14 hours
- customThe reaction was quenched with NaHCO3 (saturated)
- extractionextracted three times with ethyl acetate
- dry with materialThe organic layer was dried with magnesium sulfate
- filtrationfiltered
- customthe solvent was evaporated under reduced pressure
- customto yield crude product which
- customwas purified by silica gel chromatography (60% Ethyl acetate/heptane)