HRID509906
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)-Piperidin-3-yl-carbamic acid tert-butyl ester (2.72 g, 13.6 mmol) and 1-(3-Bromo-propyl)-3-methoxy-benzene (6.6 g, 28.8 mmol), potassium carbonate (2.5 g, 18 mmol) and sodium iodide (4 g, 26.7 mmol) are dissolved in acetonitril (40 ml) and stirred at reflux for 1 day and the solvent is removed under vacuo. The residue is taken up in dichloromethane, filtered through a pad of silica, washed with a mixture of dichloromethane: methanol:conc.ammonia=4:1:0.1 and the filtrate is evaporated. LC (method L): tR=1.30 min; Mass spectrum (ESI+): m/z=497 [M]+.
WORKUP
后处理
- temperatureat reflux for 1 day
- customthe solvent is removed under vacuo
- filtrationfiltered through a pad of silica
- washwashed with a mixture of dichloromethane
- customammonia=4:1:0.1 and the filtrate is evaporated