HRID27447

反应详情

EQUATION

反应方程式

HRID 27447 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 10.0 g of 3-benzoylacrylic acid, 1.8 g of hydrazine, and 3.7 g of potassium hydroxide in 30 ml. of aqueous ethanol (1:1) is stirred and heated at reflux for 2 hours. The cooled solution is treated with 5 ml of concentrated hydrochloric acid to pH 4.0 to precipitate 7.1 g of solid, melting point 180°-182° C. This material is dissolved in 40 ml of warm dimethylformamide and treated wit 140 ml of methanol to crystallize 3.9 g of the title compound, melting point 199°-201° C.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 2 hours
  3. customto precipitate 7.1 g of solid, melting point 180°-182° C
  4. dissolutionThis material is dissolved in 40 ml of warm dimethylformamide
  5. additiontreated wit 140 ml of methanol
  6. customto crystallize 3.9 g of the title compound, melting point 199°-201° C.