HRID1072510

反应详情

EQUATION

反应方程式

HRID 1072510 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.25 g (30 mmol) of 2,4-dichlorobenzaldehyde was introduced into 140 ml of methanol and, at room temperature, a solution of 1.71 g (30 mmol) of cyclopropylamine was added. The mixture as stirred at room temperature for 40 min and then 1.42 g (37.5 mmol) of NaBH4 was added in portions. After standing overnight, the solvent was removed and the residue was taken up in 2 N HCl. Two extractions with ethyl acetate were carried out. The aqueous phase was made alkaline with NaOH and again extracted twice with ethyl acetate. The organic phases were dried with MgSO4 and concentrated. The crude product obtained in this way, in the form of a slightly yellowish oil, was reacted further without further purification.

WORKUP

后处理

  1. waitAfter standing overnight
  2. customthe solvent was removed
  3. extractionTwo extractions with ethyl acetate
  4. extractionagain extracted twice with ethyl acetate
  5. dry with materialThe organic phases were dried with MgSO4
  6. concentrationconcentrated