HRID73851
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 stirred and heated under reflux overnight. Under reduced pressure the reaction mixture was distilled off, 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
- temperatureheated
- temperatureunder reflux overnight
- distillationUnder reduced pressure the reaction mixture was distilled off
- additionethyl acetate was 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