HRID279865

反应详情

EQUATION

反应方程式

HRID 279865 的结构方程式

PROCEDURE

实验过程

To the Compound 1a (3.1 mmol) in anhydrous methanol (8 ml) was added methyl 3-aminocrotonate (3.1 mmol) and methyl acetoacetate (3.1 mmol) and the resulting solution heated at reflux under nitrogen for 5 days. The solvent was removed in vacuo to yield a yellow oil which was purified by flash chromatography on silica gel eluted with hexane:diethyl ether (1:1) to afford Compound 1b as yellowish powder (Rf =0.3, m.p. 148°-150° C.).

WORKUP

后处理

  1. temperaturethe resulting solution heated
  2. temperatureat reflux under nitrogen for 5 days
  3. customThe solvent was removed in vacuo
  4. customto yield a yellow oil which
  5. customwas purified by flash chromatography on silica gel
  6. washeluted with hexane:diethyl ether (1:1)