HRID1835750

反应详情

EQUATION

反应方程式

HRID 1835750 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 0.5 g (2.6 mmol) of the product of Example 6 in 100 mL of toluene was added 0.8 g (5.2 mmol) of ethyl chlorooximidoacetate (Aldrich). This solution was brought to reflux and stirred for 18 hours. All solvent was removed in vacuo and the residue purified via C-18 chromatography (0-60% acetonitrile/water, 25 min.) with the product eluting at 54% acetonitrile. Concentration of the relevant fractions afforded 0.6 g (75% yield) of the title compound as a pale yellow oil.

WORKUP

后处理

  1. temperatureto reflux
  2. customAll solvent was removed in vacuo
  3. customthe residue purified via C-18 chromatography (0-60% acetonitrile/water, 25 min.) with the product
  4. washeluting at 54% acetonitrile