反応 #502134

反応方程式

methanol

ammonium chloride

trimethylaluminium

3,4-dichlorophenylacetonitrile

→

title compound

2-(3,4-Dichlorophenyl)ethanamidine hydrochloride

溶媒

toluene

toluene

反応条件

後処理

1. 1
   温度the mixture is warmed to room temperature
2. 2
   workup.STIRRINGthe mixture is stirred at 80° C. overnight
3. 3
   温度After cooling to 0° C.
4. 4
   その他The product is separated from the precipitated solid by filtration with suction
5. 5
   洗浄the filter cake is washed several times with methanol
6. 6
   その他The combined filtrates are evaporated to dryness
7. 7
   ろ過again filtered with suction

実験手順

2.88 g (54 mmol) of ammonium chloride are suspended in 50 ml of toluene under an argon atmosphere and cooled to 0° C. After dropwise addition of 27 ml of a 2 M trimethylaluminium solution in toluene, the mixture is warmed to room temperature and then stirred for 1.5 h. 5 g (27 mmol) of 3,4-dichlorophenylacetonitrile are added, and the mixture is stirred at 80° C. overnight. After cooling to 0° C., 50 ml of methanol are added dropwise. The product is separated from the precipitated solid by filtration with suction, and the filter cake is washed several times with methanol. The combined filtrates are evaporated to dryness, and the residue is then suspended in dichloromethane/methanol 10:1 and again filtered with suction. Concentration of the filtrate results in 6.2 g (77% of theory) of the title compound.

出典