HRID2261403

反应详情

EQUATION

反应方程式

HRID 2261403 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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 mmol) was dissolved in 3 ml of trifluoroacetic acid solution. Then 0.22 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 (yield: 55%) of the title compound (f).

WORKUP

后处理

  1. customThe solvent was removed in vacuo
  2. additionthe remaining residue was diluted in 20 ml of chloroform
  3. washThe organic layer was washed with 5 ml of sat. NaHCO3 solution and 5 ml of sat. NaCl solution
  4. dry with materialThen the organic layer was dried over anhydrous MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe resulting compound was purified by column chromatography on Silica gel with EtOAc solvent as an eluant