HRID1834850

反应详情

EQUATION

反应方程式

HRID 1834850 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 21.1 g. of 2-amino-4-methylbenzophenone, 58.4 g. of benzaldehyde and 35 ml. of isopropanol is added dropwise 5.5 ml. of 46% sulfuric acid while maintaining at temperature of 20°-25° C. There is then slowly added 2.7 g. of sodium borohydride while maintaining 20°-25° C. Thereafter three additional separate and alternate additions of 5.5 mls. of 46% sulfuric acid and 2.7 g. of sodium borohydride are effected while maintaining 20°-25° C. and controlling the foaming caused by the borohydride additions. After stirring for 6 hours there is added with cooling 58 g. of sodium bisulfite in 200 ml. of water followed by the addition of 100 ml. of toluene and stirring for 1.5 hours. The toluene layer is separated, washed twice with water and distilled to remove toluene and benzaldehyde. The cooled residue is treated with heptane which is flashed off and the residue cooled to obtain crystals of 2-benzylamino-4-methylbenzophenone.

WORKUP

后处理

  1. additionTo a mixture of 21.1 g
  2. customThereafter three additional separate
  3. temperaturewhile maintaining 20°-25° C.
  4. additionis added
  5. temperaturewith cooling 58 g
  6. additionof water followed by the addition of 100 ml
  7. stirringof toluene and stirring for 1.5 hours
  8. customThe toluene layer is separated
  9. washwashed twice with water
  10. distillationdistilled
  11. customto remove toluene and benzaldehyde
  12. additionThe cooled residue is treated with heptane which
  13. temperaturethe residue cooled