HRID598192

反应详情

EQUATION

反应方程式

HRID 598192 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of ethyl 2,4-dioxopentanoate (10.9 g, 68.7 mmol) and N-methoxyamine hydrochloride (4.01 g, 48.1 mmol) in ethanol (40 ml) was left to stand over molecular sieves 3A (25 g) for 18 h and diluted with dichloromethane (25 ml) The sieves was removed by filtration and the filtrate was concentrated under vacuum. The residue was purified by silica gel chromatography eluting with 5% ethyl acetate/n-hexane to give the title compound (12.9 g, 34%).

WORKUP

后处理

  1. waitwas left
  2. customwas removed by filtration
  3. concentrationthe filtrate was concentrated under vacuum
  4. customThe residue was purified by silica gel chromatography
  5. washeluting with 5% ethyl acetate/n-hexane