HRID2293648

反应详情

EQUATION

反应方程式

HRID 2293648 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

150 ml of a saturated solution of hydrogen chloride in ether are added to a solution of 149 g of 4-(tetrahydropyran-2-yloxy)-2-(3,4-dichlorophenyl)-1-aminobutane in 700 ml of methanol. The mixture is stirred for 1/2 hour at room temperature and concentrated under vacuum and the residue is taken up in 500 ml of water and washed with ether. The aqueous phase is rendered alkaline with a solution of sodium hydroxide and extracted twice with methylene chloride. The organic phases are dried over MgSO4, filtered and concentrated under vacuum. The residue is taken up in 400 ml of isopropyl ether and the mixture is stirred for one hour at room temperature. The precipitate is filtered off and washed with ether.

WORKUP

后处理

  1. concentrationconcentrated under vacuum
  2. washwashed with ether
  3. extractionextracted twice with methylene chloride
  4. dry with materialThe organic phases are dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum
  7. stirringthe mixture is stirred for one hour at room temperature
  8. filtrationThe precipitate is filtered off
  9. washwashed with ether