HRID428587
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 solution of (R)-1-benzyl-3-pyrrolidinol-tosylate (3.06 g, 9.24 mmol) in THF (30 ml) was added 1.0M solution of tetrabutylammonium fluoride in THF (37.0 ml 37.0 mmol) at room temperature. After 1.5 h stirring at reflux temperature, water (150 ml) was added to the reaction mixture and the mixture was extracted with ethyl acetate (100mix2). The combined extract was washed with water, brine, dried (Na2SO4), and concentrated to give brown oil, which was purified by column chromatography (silica gel: 80 g, CH2Cl2/MeOH 50/1) to afford 1.18 g (71%) of brown oil.
WORKUP
后处理
- additionwas added to the reaction mixture
- extractionthe mixture was extracted with ethyl acetate (100mix2)
- extractionThe combined extract
- washwas washed with water, brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated
- customto give brown oil, which
- customwas purified by column chromatography (silica gel: 80 g, CH2Cl2/MeOH 50/1)