HRID1921866

反应详情

EQUATION

反应方程式

HRID 1921866 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10.0 g (34 mmol) of methyl 2-(2-chlorobenzyloxy)-5-fluorobenzoate are dissolved in 80 ml of methanol and 40 ml of 40% strength sodium hydroxide solution and stirred at RT for 12 h. The solvent is distilled out in vacuo, water is added to the residue until it has all dissolved, and the solution is then extracted with ethyl acetate. The aqueous phase is acidified with hydrochloric acid and extracted three times with ethyl acetate. The mixture is dried over magnesium sulfate, filtered, washed with ethyl acetate and concentrated. The residue is mixed with petroleum ether, and the crystals which have separated out are filtered off with suction and dried on a clay dish. 6.00 g (21.3 mmol, 63% of theory) of the title compound are obtained.

WORKUP

后处理

  1. distillationThe solvent is distilled out in vacuo, water
  2. additionis added to the residue until it
  3. extractionthe solution is then extracted with ethyl acetate
  4. extractionextracted three times with ethyl acetate
  5. dry with materialThe mixture is dried over magnesium sulfate
  6. filtrationfiltered
  7. washwashed with ethyl acetate
  8. concentrationconcentrated
  9. additionThe residue is mixed with petroleum ether
  10. customthe crystals which have separated out
  11. filtrationare filtered off with suction
  12. customdried on a clay dish