HRID1758908

反应详情

EQUATION

反应方程式

HRID 1758908 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a 25 ml of dry chloroform, 5.4 g (0.03 m) methyl hydrogen phthalate and 3.9 g (0.033 m) thionyl chloride is added. Stir and reflux for 3 hours and cool to room temperature. To this solution 2.3 g (0.03 m) ammonium thiocyanate is added and the mixture is stirred for 3 hours at room temperature until it changed to bellow. Finally, 3.2 g (0.03 m) 2-methylaniline is added and stirred at room temperature overnight. The mixture is added to water and then some hexane is added to give fine precipitates. Filter, wash with water, hexane and dry to give 6.1 g, desired product, m.p. 143-45, yield 62%.

WORKUP

后处理

  1. temperaturereflux for 3 hours
  2. stirringthe mixture is stirred for 3 hours at room temperature until it
  3. stirringstirred at room temperature overnight
  4. customto give fine precipitates
  5. filtrationFilter
  6. washwash with water, hexane
  7. customdry