HRID567600

反应详情

EQUATION

反应方程式

HRID 567600 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of α-cyclohexylmethyl-2-piperidinobenzylamine (1.13 g, 3.96 mmol) in acetonitrile (11 ml) are added, successively, 3-ethoxy-4-ethoxycarbonyl-phenyl acetic acid (1 g, 3.96 mmol), of triphenylphosphine (1.25 g, 4.76 mmol), triethylamine (1.11 ml, 7.92 mmol) and carbon tetrachloride (0.38 ml, 3.96 mmol) and the mixture is stirred for 15 hours at ambient temperature. It is then concentrated by evaporation in vacuo and partitioned between ethyl acetate and water. The organic extract is dried and filtered and concentrated by evaporation in vacuo. The evaporation residue is purified by column chromatography on silica gel (toluene/acetone=10/1).

WORKUP

后处理

  1. concentrationIt is then concentrated by evaporation in vacuo
  2. custompartitioned between ethyl acetate and water
  3. extractionThe organic extract
  4. customis dried
  5. filtrationfiltered
  6. concentrationconcentrated by evaporation in vacuo
  7. customThe evaporation residue is purified by column chromatography on silica gel (toluene/acetone=10/1)