HRID277631

反应详情

EQUATION

反应方程式

HRID 277631 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

11.9 g (0.032 mol) of 1-benzyloxy-2-methyl-4-benzoyloxynaphthalene was suspended in 120 ml of methanol, and to this was added 20 ml of 2N NaOH, followed by stirring for 2 hours at room temperature. After evaporation of methanol from the reaction mixture under reduced pressure, the residue was acidified with hydrochloric acid, and extracted with ethyl acetate. The organic layer was washed with a sodium hydrogen carbonate aqueous solution and then with water, and ethyl acetate evaporated under reduced pressure. The residue was dissolved in methanol, decolorized with activated carbon, and following filtering out of the activated carbon, water was added to the filtrate, and precipitated crystals were collected, recrystallized from methanol-water to give 5.2 g of white plates, m.p. 159-161° C.

WORKUP

后处理

  1. customAfter evaporation of methanol from the reaction mixture under reduced pressure
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with a sodium hydrogen carbonate aqueous solution
  4. customwith water, and ethyl acetate evaporated under reduced pressure
  5. dissolutionThe residue was dissolved in methanol
  6. filtrationfollowing filtering out of the activated carbon, water
  7. additionwas added to the filtrate
  8. customprecipitated crystals
  9. customwere collected
  10. customrecrystallized from methanol-water
  11. customto give 5.2 g of white plates, m.p. 159-161° C.