HRID731249

反应详情

EQUATION

反应方程式

HRID 731249 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A solution of 2-oxo-cyclopentanecarboxylic acid ethyl ester (5.00 g, 32.0 mmol) in ethanol (50 mL) was treated with N,N-dimethylethylenediamine (3.85 mL, 35.2 mmol). The solution was heated at reflux at 80° C. for 16 h. After cooling to 25° C. the solvent was removed in vacuo, and the residue was purified by flash column chromatography (Teledyne Isco RediSep Flash Column 40 g; 0-100% ethyl acetate in hexanes) to afford the desired product, 2-(2-dimethylamino-ethylamino)-cyclopent-1-enecarboxylic acid ethyl ester (6.7 g, 29.6 mmol, 92.5%), as a light yellow oil. The product was used immediately in the following step without characterization.

WORKUP

后处理

  1. temperatureThe solution was heated
  2. temperatureAfter cooling to 25° C. the solvent
  3. customwas removed in vacuo
  4. customthe residue was purified by flash column chromatography (Teledyne Isco RediSep Flash Column 40 g; 0-100% ethyl acetate in hexanes)