HRID220231

反应详情

EQUATION

反应方程式

HRID 220231 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3.03 g of crude 5-hydroxy-5-(4-methoxy-phenyl)-bicyclo[2.2.2]octan-2-one (intermediate K2A.1) was dissolved in 100 mL of acetone, 2.90 g of TsOH were added and the mixture was stirred at rt overnight. Then the reaction mixture was diluted with EtOAc, the organic phase washed with sat. aq. NaHCO3 and evaporated. The crude material was purified by CC with Hep-EtOAc (20:1) to yield 2.36 g of rac-(1R*,4R*)-5-(4-methoxy-phenyl)-bicyclo[2.2.2]oct-5-en-2-one.

WORKUP

后处理

  1. washthe organic phase washed with sat. aq. NaHCO3
  2. customevaporated
  3. customThe crude material was purified by CC with Hep-EtOAc (20:1)