HRID1069199

反应详情

EQUATION

反应方程式

HRID 1069199 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3.2 g (12.1 mmol) of methyl 2-benzyloxyimino-3-methoxyiminobutyrate in 50 ml of methanol, 1.01 g (24.2 mmol) of sodium hydroxide and 10 ml of water were added and the mixture was heated under reflux for 24 hours. After distilling the solvent off under reduced pressure and adding 50 ml of water, the mixture was washed with 50 ml of diethylether. The aqueous layer was made acidic by adding a concentrated hydrochloric acid, and then the mixture was extracted three times with 50 ml of diethylether. After washing with water and with a saturated aqueous sodium chloride, the organic layer was dried over with anhydrous magnesium sulfate and the solvent was distilled off to obtain 3.02 g (yield: 100% ) of 2-benzyloxyimino-3-methoxyiminobutyric acid as a white solid.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 24 hours
  3. distillationAfter distilling the solvent off under reduced pressure
  4. additionadding 50 ml of water
  5. washthe mixture was washed with 50 ml of diethylether
  6. additionby adding a concentrated hydrochloric acid
  7. extractionthe mixture was extracted three times with 50 ml of diethylether
  8. washAfter washing with water and with a saturated aqueous sodium chloride
  9. dry with materialthe organic layer was dried over with anhydrous magnesium sulfate
  10. distillationthe solvent was distilled off