反应 #1269893

反应方程式

5-chloro-2-nitrobenzyl alcohol

triethylamine

thionyl chloride

→

title compound

收率 99.0%

4-Chloro-2-chloromethyl-1-nitro-benzene

收率 99.0%

溶剂

dichloromethane

反应条件

后处理

1. 1
   其他was kept below 32° C.
2. 2
   温度by cooling with a water bath
3. 3
   其他The solvent was evaporated
4. 4
   其他the residue was triturated in warm tert-butyl methyl ether (970 ml)
5. 5
   其他The ammonium salts were removed by filtration
6. 6
   浓缩the filtrate was concentrated in vacuo

实验过程

To a solution of 5-chloro-2-nitrobenzyl alcohol (80 g, 0.42 mol) and triethylamine (64 ml, 0.46 mol) in dichloromethane (840 ml) was added drop wise thionyl chloride (34 ml, 0.46 mol) during a period of 30 min while the internal temperature was kept below 32° C. by cooling with a water bath. The reaction mixture was stirred for 3 h. The solvent was evaporated and the residue was triturated in warm tert-butyl methyl ether (970 ml). The ammonium salts were removed by filtration and the filtrate was concentrated in vacuo to give the title compound (85 g, 99%) as brown oil which was used in the next step without purification. MS m/e: 205 (M+).

来源