HRID652963

反应详情

EQUATION

反应方程式

HRID 652963 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 620 mg (2 mmol) of the piperazine derivative in dry tetrahydrofuran (5 ml) was added a solution of 766 mg (2.0 mmol) of N-[3-[3-methoxy-4-(β-methoxyethoxymethoxy)phenyl]-2-propenoyl) thiazolidine-2-thione in dry tetrahydrofuran (5 ml), and the mixture was allowed to react at room temperature overnight under argon atmosphere. The reaction mixture was concentrated by evaporation under reduced pressure, diluted with N'chloroform and washed, in turn, with 2N aqueous solution of sodium hydroxide and water. The organic layer was dried over anhydrous scdium sulfate and concentrated by evaporation under reduced pressure. The residue was subjected to silica gel column chromatography, eluted with chloroform - methanol ((50 : 1), to give 1.08 g (1.88 mmol) of N-[3-[3-methoxy-4-(β-methoxyethoxymetoxy) phenyl]-2-propenoyl]-N'-(3-benzhydroxypropyl)-piperazine.

WORKUP

后处理

  1. customto react at room temperature overnight under argon atmosphere
  2. concentrationThe reaction mixture was concentrated by evaporation under reduced pressure
  3. additiondiluted with N'chloroform
  4. washwashed, in turn, with 2N aqueous solution of sodium hydroxide and water
  5. dry with materialThe organic layer was dried over anhydrous scdium sulfate
  6. concentrationconcentrated by evaporation under reduced pressure
  7. washeluted with chloroform - methanol ((50 : 1)