HRID865393
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
To a solution of 80 ml THF, 40 ml water, and 800 mg oxalic acid was added 9.6 g (40 mmol) of N-benzyloxycarbonyl aminoacetaldehyde dimethyl acetal, and refluxed for 4 days. The THF was removed under reduced pressure and the remaining solution was extracted with ether (3×100 ml), the ether fractions were combined and dried over anhydrous sodium sulfate. The ether was removed under reduced pressure and the remaining solution was purified by flash chromatography (hexane and ethyl acetate 3:1 then 1:1) to yield 3.88 g, 50% yield.
WORKUP
后处理
- temperaturerefluxed for 4 days
- customThe THF was removed under reduced pressure
- extractionthe remaining solution was extracted with ether (3×100 ml)
- dry with materialdried over anhydrous sodium sulfate
- customThe ether was removed under reduced pressure
- customthe remaining solution was purified by flash chromatography (hexane and ethyl acetate 3:1
- custom1:1) to yield 3.88 g, 50% yield