HRID1833237

反应详情

EQUATION

反应方程式

HRID 1833237 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
1110 °C

PROCEDURE

实验过程

To a stirred solution of 2-(3,4-dimethoxy-phenyl)-3-oxo-propionitrile (26 g, 127 mmol) in toluene ((275 mL) was added ethyl carbamate (11.3 g, 127 mmol) and concentrated sulfuric acid solution (2.0 mL). The reaction mixture was heated at 1110° C. with a Dean-Stark apparatus. The mixture was cooled and a solid was precipitated. The mixture was filtered and the solid was collected. The yellow solid was washed with diethyl ether to afford [2-cyano-2-(3,4-dimethoxy-phenyl)-vinyl]-carbamic acid ethyl ester (20 g, 57% yield).

WORKUP

后处理

  1. temperatureThe mixture was cooled
  2. customa solid was precipitated
  3. filtrationThe mixture was filtered
  4. customthe solid was collected
  5. washThe yellow solid was washed with diethyl ether