HRID1533033

反应详情

EQUATION

反应方程式

HRID 1533033 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Ethyl 2-(1-benzyl-4-(3,5-dimethylphenyl)piperidin-4-yl)ethanoate (2.0 g) (see Preparation 9) was dissolved in anhydrous diethyl ether (50 ml), cooled in an ice-bath and lithium aluminium hydride (0.21 g) added portionwise. The mixture was stirred at room temperature for 45 minutes, water (0.3 ml) was carefully added, followed by 2N aqueous sodium hydroxide solution (0.3 ml) and fiiter water (0.6 ml). The mixture was stirred for 20 minutes and the resulting granular precipitate removed by filtration and washed with diethyl ether. The solvent was removed from the filtrate under reduced pressure to give a solid which was dissolved in dichloromethane, dried over anhydrous sodium sulphate and the solvent again removed under reduced pressure to yield 4-(3,5-dimethylphenyl)-4-(2-hydroxyethyl)-N-benzylpiperidine (1.67 g) as an oil.

WORKUP

后处理

  1. temperaturecooled in an ice-bath
  2. stirringThe mixture was stirred for 20 minutes
  3. customthe resulting granular precipitate removed by filtration
  4. washwashed with diethyl ether
  5. customThe solvent was removed from the filtrate under reduced pressure
  6. customto give a solid which
  7. dry with materialdried over anhydrous sodium sulphate
  8. customthe solvent again removed under reduced pressure