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
- -15 °C
PROCEDURE
实验过程
Yet alternatively, 0.67 g 4-nitrophenol are dissolved in 5 mL ethanol. 4.6 mL of 1 M aqueous sodium hydroxide solution are added. The mixture is cooled to −15° C. A solution of 1.0 g 2,4-dichloro-5-trifluoromethylpyrimidine in 2 mL ethanol is added at −15° C. in portions. The suspension is stirred for 1.5 hours at −15° C. to −10° C. and then warmed up to 20° C. during 3 hours. The suspension is stirred 16 hours at 20° C. The precipitate is filtered and washed with a 1:1-mixture of methanol and purified water. The product is dried in a vacuum drying oven. 1.3 g (88% of theory) of title product is obtained with a regioisomeric purity of 88:12 (2-chloro-4-(4-nitrophenyloxy)-5-trifluoromethylpyrimidine:2-(4-nitrophenyloxy)-4-chloro-5-trifluoromethylpyrimidine).
WORKUP
后处理
- temperaturewarmed up to 20° C. during 3 hours
- stirringThe suspension is stirred 16 hours at 20° C
- filtrationThe precipitate is filtered
- washwashed with a 1
- custom1-mixture of methanol and purified water
- customThe product is dried in a vacuum
- customdrying oven