HRID53637

反应详情

EQUATION

反应方程式

HRID 53637 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-Piperidinylmethyl 8-amino-7-chloro-1,4-benzodioxan-5-carboxylate (0.100 g; 10.31 mmol) was dissolved in acetone (10 ml) and treated with triethylamine (0.043 ml; 0.31 mmol) and methyl vinyl ketone (0.026 ml; 0.34 mmol). The solution was heated at reflux (18 hours), cooled and evaporated in vacuo to a yellow gum. The gum was purified by flash silica-gel chromatography with CHCl3 as eluant to yield the title compound as a colourless gum (0.050 g; 41%) which was converted to the oxalate salt.

WORKUP

后处理

  1. temperatureThe solution was heated
  2. temperatureat reflux (18 hours)
  3. temperaturecooled
  4. customevaporated in vacuo to a yellow gum
  5. customThe gum was purified by flash silica-gel chromatography with CHCl3 as eluant