HRID387192

反应详情

EQUATION

反应方程式

HRID 387192 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
82 °C

PROCEDURE

实验过程

2-Methoxy-5-trifluoromethylphenyl isocyanate (1057.8 g) is dissolved in acetonitrile (4240 ml), then 2-fluoroaniline (540.8 g) is added thereto and the mixture is rinsed in with acetonitrile (50 ml). The resulting clear solution is stirred under reflux (ca. 82° C.) for 4 h, then seeded at ca. 78° C. and stirred for ca. 15 min. The suspension is cooled to 0° C., and the product is filtered off with suction and washed with acetonitrile (950 ml, cooled to 0-5° C.). The product is dried overnight at 45° C. in a vacuum drying oven using entraining nitrogen. A total of 1380.8 g of N-(2-fluorophenyl)-N′-[2-methoxy-5-(trifluoromethyl)phenyl]urea are obtained as a solid, corresponding to 86.4% of theory.

WORKUP

后处理

  1. washthe mixture is rinsed in with acetonitrile (50 ml)
  2. customseeded at ca. 78° C.
  3. stirringstirred for ca. 15 min
  4. temperatureThe suspension is cooled to 0° C.
  5. filtrationthe product is filtered off with suction
  6. washwashed with acetonitrile (950 ml, cooled to 0-5° C.)
  7. customThe product is dried overnight at 45° C. in a vacuum
  8. customdrying oven