HRID441898

反应详情

EQUATION

反应方程式

HRID 441898 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

15.1 g. of phenyl N-methylcarbamate, 9.3 g. of aniline and 5.4 g. of tetraethylammonium salt of 2-hydroxy-5-nitro-pyridine are refluxed in 200 ml. of ethanol for 5 hours. The reaction solution is concentrated, and the residue is dissolved in 100 ml. of chloroform, washed successively with 50 ml. of 1N sodium carbonate, 50 ml. of 1N hydrochloric acid and 100 ml. of water, and dried. By concentrating to dryness and recrystallizing from 120 ml. of ethanol, crystals of N-methyl-N-phenylurea having a m.p. of 150° - 151° C. are obtained in 91 percent yield.

WORKUP

后处理

  1. concentrationThe reaction solution is concentrated
  2. dissolutionthe residue is dissolved in 100 ml
  3. washof chloroform, washed successively with 50 ml
  4. dry with materialof water, and dried
  5. concentrationBy concentrating to dryness
  6. customrecrystallizing from 120 ml