HRID1851831

反应详情

EQUATION

反应方程式

HRID 1851831 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10 ml of N-methylmorpholine was added to 1.0 g (9.1 mmol) of L-valine and 2.0 g (9.1 mmol) of 2-(2-furanyl)-3-oxa-1-azaspiro[4.5]dec-1-en-4-one, and the mixture was refluxed under heating overnight. The reaction solution was distilled off under reduced pressure, ethyl acetate was added thereto, and the mixture was washed with a 10% aqueous potassium hydrogensulfate solution and then saturated brine, followed by drying with anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the residue was purified by silica gel chromatography to obtain 384 mg (12.5%) of the title compound.

WORKUP

后处理

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating overnight
  3. distillationThe reaction solution was distilled off under reduced pressure, ethyl acetate
  4. additionwas added
  5. washthe mixture was washed with a 10% aqueous potassium hydrogensulfate solution
  6. dry with materialby drying with anhydrous sodium sulfate
  7. distillationThe solvent was distilled off under reduced pressure
  8. customthe residue was purified by silica gel chromatography