反应 #586152

反应方程式

nitric acid

1-chloro-3-(2,6-dichloro-4-trifluoromethylphenyl)benzene

→

1-chloro-5-(2,6-dichloro-4-trifluoromethylphenyl)-2-nitrobenzene

收率 52.6%

溶剂

反应条件

后处理

1. 1
   萃取extracted with 100 ml of diethyl ether twice
2. 2
   洗涤The diethyl ether layer was washed with 200 ml of water twice
3. 3
   干燥dried over anhydrous magnesium sulfate
4. 4
   workup.DISTILLATIONthe diethyl ether was distilled off under reduced pressure
5. 5
   其他Purification of the residue by silica gel column chromatography

实验过程

To 50 ml of fuming nitric acid, 5.0 g (15.4 mmol) of 1-chloro-3-(2,6-dichloro-4-trifluoromethylphenyl)benzene was added dropwise at −30° C. After 15 minutes of stirring at the same temperature, the reaction mixture was warmed to 5° C., poured into about 200 ml of ice-cold water and extracted with 100 ml of diethyl ether twice. The diethyl ether layer was washed with 200 ml of water twice and dried over anhydrous magnesium sulfate, and the diethyl ether was distilled off under reduced pressure. Purification of the residue by silica gel column chromatography afforded 3.0 g of 1-chloro-5-(2,6-dichloro-4-trifluoromethylphenyl)-2-nitrobenzene (yield 52.6%) as a pale yellow liquid (nD20 1.5744), which was used in Example 8 (2) as the starting material.

来源