HRID880352

反应详情

EQUATION

反应方程式

HRID 880352 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred solution of ethyl 4-[2,4-bis(benzyloxy)-6-(4-nitrophenoxy)phenyl]-2,4-dioxobutanoate (5 g, 9 mmol) and hydroxylamine hydrochloride (0.74 g, 15 mmol, 1.2 eq) in ethanol (mL 50) was refluxed for 2 hours. The solution was concentrated to a small volume and diluted with ethyl acetate. After washing with brine and drying, the solvent was removed and the residue was carefully chromatographed on silica gel eluting with hexane/ethyl acetate 6/1, to provide the title compound (4.1 g, 82% yield).

WORKUP

后处理

  1. concentrationThe solution was concentrated to a small volume
  2. additiondiluted with ethyl acetate
  3. washAfter washing with brine
  4. customdrying
  5. customthe solvent was removed
  6. customthe residue was carefully chromatographed on silica gel eluting with hexane/ethyl acetate 6/1