HRID1862572

反应详情

EQUATION

反应方程式

HRID 1862572 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In 200 ml of methanol, were dissolved 2.00 g of the compound obtained in Example 11, 0.86 ml of methyl orthoformate and 0.004 g of p-toluenesulfonic acid monohydrate. The resulting solution was refluxed for 12 hours. After completing the reaction, 0.03 ml of triethylamine was added to the reaction solution, and the solvent was then removed under reduced pressure. Ethyl acetate was added to the residue, and the resulting solution was extracted with ethyl acetate. The organic layer was dried over sodium sulfate. The solvent was removed under reduced pressure to provide 2.35 g (quantitatively) of the title compound.

WORKUP

后处理

  1. temperatureThe resulting solution was refluxed for 12 hours
  2. additionwas added to the reaction solution
  3. customthe solvent was then removed under reduced pressure
  4. additionEthyl acetate was added to the residue
  5. extractionthe resulting solution was extracted with ethyl acetate
  6. dry with materialThe organic layer was dried over sodium sulfate
  7. customThe solvent was removed under reduced pressure