HRID1390334

反应详情

EQUATION

反应方程式

HRID 1390334 的结构方程式

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

To a mixture of 35.2 g. (0.11 mole) of 5-[bis-(4-chlorophenyl)-methyl]-2-pyridone and 11.8 g. (0.11 mole) of 2,4-lutidine, add 50.6 g. (0.33 mole) of phosphorous oxychloride (dropwise) while heating the reaction mixture at 80°. Then, heat the reaction mixture at 120° C. for six hours. Pour the reaction mixture onto ice, basify with ammonium hydroxide, extract with benzene and remove both the benzene and residual 2,4-lutidine by distillation. Distill the residue at about 195°-210° C. (0.01 mm) to obtain thereby about 30 g. of the product of this step as a yellow viscous oil.

WORKUP

后处理

  1. additionTo a mixture of 35.2 g
  2. additionPour the reaction mixture onto ice
  3. extractionextract with benzene
  4. customremove both the benzene and residual 2,4-lutidine
  5. distillationby distillation
  6. distillationDistill the residue at about 195°-210° C. (0.01 mm)
  7. customto obtain