HRID1437233
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
Under cooling with ice, pyridinesulfonic acid (19.7 g) in dimethyl sulfoxide (84 mL) was added dropwise to 1-benzhydrylazetidin-3-ol (4.79 g) in triethylamine (27.9 mL), and the resultant mixture was stirred at 50° C. for 40 minutes. The reaction mixture was partitioned between ice-water and ethyl acetate. The organic layer was washed with saturated brine, and then dried over magnesium sulfate anhydrate, followed by filtration. The solvent was evaporated under reduced pressure. The residue was purified through silica gel column chromatography (hexane-ethyl acetate), to thereby give the title compound as a solid (2.85 g, 60%).
WORKUP
后处理
- customThe reaction mixture was partitioned between ice-water and ethyl acetate
- washThe organic layer was washed with saturated brine
- dry with materialdried over magnesium sulfate anhydrate
- filtrationfollowed by filtration
- customThe solvent was evaporated under reduced pressure
- customThe residue was purified through silica gel column chromatography (hexane-ethyl acetate)