HRID973165

反应详情

EQUATION

反应方程式

HRID 973165 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 87.5 g (0.39 mole) of 4'-phenethylacetophenone, M.P. 67°-70° C., prepared according to R. E. Lutz et al., J. Org. Chem. 12, 617 (1947), and 98.5 g (1.56 mole) of ammonium formate is slowly heated to 150° C. with stirring. After the initial foaming has subsided the temperature of the heating bath is raised to 185°-190° C. for a period of 4 hours. Upon cooling, the mixture is treated with several portions of water. To the residue is added 75 ml of concentrated HCl. The mixture is refluxed for 2 hours and is allowed to cool. The resulting solid is collected, washed with several portions of benzene and is recrystallized from isopropanol containing about 5% of water to yield 74.0 g (73% yield) of the desired product, M.P. 212°-214° C.

WORKUP

后处理

  1. customprepared
  2. temperatureis raised to 185°-190° C. for a period of 4 hours
  3. temperatureUpon cooling
  4. temperatureThe mixture is refluxed for 2 hours
  5. temperatureto cool
  6. customThe resulting solid is collected
  7. washwashed with several portions of benzene
  8. customis recrystallized from isopropanol containing about 5% of water