HRID274433

反应详情

EQUATION

反应方程式

HRID 274433 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

ba) 3.2 g of alpha-[4-(benzyloxy)-5-methoxyphenyl]-3-pyridinemethanol suspended in 50 ml of water are treated with 2.5 g of potassium permanganate, whereupon the mixture is stirred at 90° for 30 minutes After adding a further 1.0 g of potassium permanganate and stirring for a further 30 minutes at 90° the mixture is cooled to room temperature and extracted twice with 150 ml of ethyl acetate each time. The combined ethyl acetate phases are washed with sodium chloride solution, dried over sodium sulfate and evaporated. The thus-obtained residue is chromatographed on 50 g of silica gel with ethyl acetate. After recrystallization from methylene chloride/hexane there is obtained 4-(benzyloxy)-3-methoxyphenyl 3-pyridyl ketone of m.p. 76°.

WORKUP

后处理

  1. stirringstirring for a further 30 minutes at 90° the mixture
  2. extractionextracted twice with 150 ml of ethyl acetate each time
  3. washThe combined ethyl acetate phases are washed with sodium chloride solution
  4. dry with materialdried over sodium sulfate
  5. customevaporated
  6. customThe thus-obtained residue is chromatographed on 50 g of silica gel with ethyl acetate
  7. customAfter recrystallization from methylene chloride/hexane there