HRID442852

反应详情

EQUATION

反应方程式

HRID 442852 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Compound 1 (1.43 g, 2.28 mmol) obtained in Example 1 was dissolved in a mixed solvent of tetrahydrofuran (20 ml) and ethanol (20 ml), and 5 ml of 2N hydrochloric acid was added thereto, followed by heating under reflux for 0.5 hours. The solvent was distilled off under reduced pressure, and a saturated aqueous solution of sodium bicarbonate was added thereto followed by extraction with ethyl acetate. The resulting organic layer was washed with a saturated aqueous solution of sodium chloride and dried over magnesium sulfate, and the solvent was distilled off under pressure. The resulting residue was washed with diethyl ether/ethyl acetate and crystallized to give 1.1 g (yield: 88%) of the title compound.

WORKUP

后处理

  1. additionwas added
  2. temperatureby heating
  3. temperatureunder reflux for 0.5 hours
  4. distillationThe solvent was distilled off under reduced pressure
  5. additiona saturated aqueous solution of sodium bicarbonate was added
  6. extractionthereto followed by extraction with ethyl acetate
  7. washThe resulting organic layer was washed with a saturated aqueous solution of sodium chloride
  8. dry with materialdried over magnesium sulfate
  9. distillationthe solvent was distilled off under pressure
  10. washThe resulting residue was washed with diethyl ether/ethyl acetate
  11. customcrystallized