HRID1609062

反应详情

EQUATION

反应方程式

HRID 1609062 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

11 g of the compound (123) obtained in Comparative Example 5 was added to 200 ml of concentrated hydrochloric acid, and the solution heated at reflux for 2.5 hours. After air-cooling, the solution was extracted with 500 ml of ethyl acetate four times, and the extract was washed with aqueous 10% sodium hydrogen carbonate solution. After drying over magnesium sulfate, the solvent was removed by distillation. The residue was crystallized with n-hexane, and the crystals were filtered to obtain 8.33 g of the subject compound (124) in a 97% yield.

WORKUP

后处理

  1. temperaturethe solution heated
  2. temperatureat reflux for 2.5 hours
  3. temperatureAfter air-cooling
  4. extractionthe solution was extracted with 500 ml of ethyl acetate four times
  5. washthe extract was washed with aqueous 10% sodium hydrogen carbonate solution
  6. dry with materialAfter drying over magnesium sulfate
  7. customthe solvent was removed by distillation
  8. customThe residue was crystallized with n-hexane
  9. filtrationthe crystals were filtered