HRID1851831
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe mixture was refluxed
- temperatureunder heating overnight
- distillationThe reaction solution was distilled off under reduced pressure, ethyl acetate
- additionwas added
- washthe mixture was washed with a 10% aqueous potassium hydrogensulfate solution
- dry with materialby drying with anhydrous sodium sulfate
- distillationThe solvent was distilled off under reduced pressure
- customthe residue was purified by silica gel chromatography