HRID1597269

反应详情

EQUATION

反应方程式

HRID 1597269 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-70 °C

PROCEDURE

实验过程

A solution of 15 g of 2-bromoanisole in 50 ml of THF is cooled to −70° C., under nitrogen, a 1.6 M solution of n-butyllithium in THF is added dropwise and the mixture is kept stirring for 1 hour. The mixture is cooled to −70° C. and a solution of 15.2 g of 1-benzylpiperid-4-one in 50 ml of THF is added dropwise. The mixture is kept stirring while allowing the temperature to rise to RT and after 1 hour, the reaction mixture is concentrated under vacuum. The residue is taken up in AcOEt, the organic phase washed with water, with a saturated solution of NaCl, dried over MgSO4 and the solvent evaporated under vacuum. 14 g of the expected product are obtained after crystallization from the AcOEt/ether/heptane mixture.

WORKUP

后处理

  1. stirringThe mixture is kept stirring
  2. waitto rise to RT and after 1 hour
  3. concentrationthe reaction mixture is concentrated under vacuum
  4. washthe organic phase washed with water, with a saturated solution of NaCl
  5. dry with materialdried over MgSO4
  6. customthe solvent evaporated under vacuum