HRID1609726

反应详情

EQUATION

反应方程式

HRID 1609726 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 5.12 g (13.0 mmol) of (4-fluorophenyl)[2-methoxy-5-(2,6-dimethyl-4nitrophenoxy) phenyl]methanone in 100 ml methylene chloride is chilled in an ice bath and 40 ml (40 mmol) of 1.0 M boron trichloride in methylene chloride is gradually added. The solution is stirred at room temperature overnight, then poured into 300 ml of ice water and stirred 2 hours. The organic layer is separated, washed with 5% aqueous sodium carbonate, water, dried (CaSO4) and evaporated. The residue is recrystallized from ethanol to give (4-fluorophenyl)[2-hydroxy-5-(2,6-dimethyl-4 nitrophenoxy)phenyl]methanone, m.p. 148°-150°.

WORKUP

后处理

  1. stirringstirred 2 hours
  2. customThe organic layer is separated
  3. washwashed with 5% aqueous sodium carbonate, water
  4. dry with materialdried (CaSO4)
  5. customevaporated
  6. customThe residue is recrystallized from ethanol