HRID443023
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
3-(t-Butoxycarbonylamino)propanol (10.0 g) is dissolved in methylene chloride (100 ml), and thereto are added with stirring triethylamine (8.66 g) and tosyl chloride (16.3 g) under ice-cooling, and the reaction mixture is stirred at room temperature overnight. The reaction mixture is concentrated, and the residue is dissolved in a mixture of water and ethyl acetate. The organic layer is separated, washed with a saturated sodium chloride solution, dried over sodium sulfate, and concentrated under reduced pressure. The residue is purified by silica gel column chromatography to give the title compound (15.37 g) as a pale yellow oil.
WORKUP
后处理
- temperaturecooling
- concentrationThe reaction mixture is concentrated
- dissolutionthe residue is dissolved in a mixture of water and ethyl acetate
- customThe organic layer is separated
- washwashed with a saturated sodium chloride solution
- dry with materialdried over sodium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue is purified by silica gel column chromatography