HRID363094

反应详情

EQUATION

反应方程式

HRID 363094 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 2.87 g of 1-benzoyloxy-4-(2-chlorobenzyloxy)-3,5-dichlorobenzene and 100 ml of methanol was added dropwise 5.1 g of 10% (w/w) aqueous potassium hydroxide solution, while stirring at room temperature. After stirring at room temperature for 6 hours, the reaction mixture was made weakly acidic by the addition of 10% hydrochloric acid, and the methanol was removed by distillation under reduced pressure. The residue was extracted twice with 100 ml of ethyl acetate. The combined ether layer was washed with water, and dried with anhydrous magnesium sulfate, followed by removal of the solvent by distillation under reduced pressure. The residue was subjected to silica gel chromatography, which afforded 1.17 g of 4-(2-chlorobenzyloxy)-3,5-dichlorophenol (55% yield), m.p. 108.3° C.

WORKUP

后处理

  1. stirringAfter stirring at room temperature for 6 hours
  2. customthe methanol was removed by distillation under reduced pressure
  3. extractionThe residue was extracted twice with 100 ml of ethyl acetate
  4. washThe combined ether layer was washed with water
  5. dry with materialdried with anhydrous magnesium sulfate
  6. customfollowed by removal of the solvent by distillation under reduced pressure