HRID77508
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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
A mixture of 4-bromomethyl-benzoic acid methyl ester (3.0 g; 15 mmol), piperidin-4-yl-carbamic acid tert-butyl ester (3.77 g; 16.5 mmol) and potassium carbonate (4.35 g, 31.5 mmol) in 100 ml acetonitrile is stirred for 5 h at 80° C. Precipitates were removed by filtration and the solution is evaporated. The residue is purified by silica gel column chromatography (gradient: DCM/Methanol 98:2 to 95:5 to yield 4-(4-tert-Butoxycarbonylamino-piperidin-1-ylmethyl)-benzoic acid methyl ester.
WORKUP
后处理
- customPrecipitates
- customwere removed by filtration
- customthe solution is evaporated
- customThe residue is purified by silica gel column chromatography (gradient