HRID1833237
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe mixture was cooled
- customa solid was precipitated
- filtrationThe mixture was filtered
- customthe solid was collected
- washThe yellow solid was washed with diethyl ether