HRID865393

反应详情

EQUATION

反应方程式

HRID 865393 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 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

  1. temperaturerefluxed for 4 days
  2. customThe THF was removed under reduced pressure
  3. extractionthe remaining solution was extracted with ether (3×100 ml)
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe ether was removed under reduced pressure
  6. customthe remaining solution was purified by flash chromatography (hexane and ethyl acetate 3:1
  7. custom1:1) to yield 3.88 g, 50% yield