HRID441898
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- concentrationThe reaction solution is concentrated
- dissolutionthe residue is dissolved in 100 ml
- washof chloroform, washed successively with 50 ml
- dry with materialof water, and dried
- concentrationBy concentrating to dryness
- customrecrystallizing from 120 ml