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