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
310 mg of 3-[1-(2,4-dimethoxybenzyl)-2-oxo-1,2,5,6-tetrahydro-pyridin-3-yl]-propionic acid methyl ester (d) (0.93 mM) was dissolved in 3 ml of trifluoroacetic acid solution. Then 0.222 ml of triethyl silane (1.395 mmol) was added thereto and the mixture was heated for 20 min at 80° C. The solvent was removed in vacuo and the remaining residue was diluted in 20 ml of chloroform. The organic layer was washed with 5 ml of sat. NaHCO3 solution and 5 ml of sat. NaCl solution. Then the organic layer was dried over anhydrous MgSO4, filtered and concentrated in vacuo. The resulting compound was purified by column chromatography on Silica gel with EtOAc solvent as an eluant to give 126 mg of the title compound (f) (yield: 55%).
WORKUP
后处理
- customThe solvent was removed in vacuo
- additionthe remaining residue was diluted in 20 ml of chloroform
- washThe organic layer was washed with 5 ml of sat. NaHCO3 solution and 5 ml of sat. NaCl solution
- dry with materialThen the organic layer was dried over anhydrous MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe resulting compound was purified by column chromatography on Silica gel with EtOAc solvent as an eluant