HRID1478603
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
(S)-tert-butyl 3-(hydroxymethyl)piperidine-1-carboxylate (3.5 g, 16.59 mmol) was dissolved in CH2Cl2 (60 ml), and then TsCl (3.8 g, 19.91 mmol), Et3N (3.47 ml, 24.87 mmol), and DMAP (0.21 g, 1.66 mmol) were added, followed by at room temperature for 3 hours. After the completion of the reaction, the reaction mixture was extracted with H2O, MC, and brine, followed by drying (Na2SO4), filtration, and concentration under reduced pressure, and the residue was purified by column chromatography (EA:Hex=1:5), to give (S)-tert-butyl 3-((tosyloxy)methyl)piperidine-1-carboxylate (6 g, 97%).
WORKUP
后处理
- customAfter the completion of the reaction
- extractionthe reaction mixture was extracted with H2O, MC, and brine
- customby drying
- filtration(Na2SO4), filtration, and concentration under reduced pressure
- customthe residue was purified by column chromatography (EA:Hex=1:5)