反应 #4359

反应方程式

nitric acid

sulphuric acid

2,4-dichloro-5-fluorobenzoic acid

→

2,4-dichloro-5-fluoro-3-nitro-benzoic acid

溶剂

反应条件

后处理

1. 1
   温度while cooling with ice
2. 2
   其他rises to 45°-50° C
3. 3
   温度The mixture is then heated at 90°-100° C. for a further 3 hours
4. 4
   过滤the precipitate is filtered off with suction
5. 5
   洗涤washed with water
6. 6
   workup.DISSOLUTIONThe moist crude product is dissolved hot in 30 ml of methanol
7. 7
   workup.ADDITION150 ml of H2O were added to the solution
8. 8
   过滤The precipitate is filtered off cold with suction
9. 9
   洗涤washed with CH3OH/H2O
10. 10
    其他dried in vacuo at 80° C

实验过程

40 ml of concentrated nitric acid are added dropwise to 34 ml of concentrated sulphuric acid, while cooling with ice and stirring. 20.9 g of 2,4-dichloro-5-fluorobenzoic acid are introduced in portions into this nitration mixture, whereupon the temperature rises to 45°-50° C. The mixture is then heated at 90°-100° C. for a further 3 hours, the mixture is cooled to room temperature and poured onto 350 ml of ice-water and the precipitate is filtered off with suction and washed with water. The moist crude product is dissolved hot in 30 ml of methanol, and 150 ml of H2O were added to the solution. The precipitate is filtered off cold with suction, washed with CH3OH/H2O and dried in vacuo at 80° C. 21.2 g of crude 2,4-dichloro-5-fluoro-3-nitro-benzoic acid are obtained. The compound is sufficiently pure for the subsequent reactions. A sample recrystallized from toluene/petroleum ether gives crystals of melting point 192° C.

来源