反応 #218510

反応方程式

2,4-difluoro-1-nitro-benzene

2-amino-5-trifluoromethyl-benzonitrile

lithium hydroxide monohydrate

→

title compound

収率 96.0%

2-(5-Fluoro-2-nitro-phenylamino)-5-trifluoromethyl-benzonitrile

収率 96.0%

溶媒

methyl sulfoxide

反応条件

後処理

1. 1
   温度Cool the reaction mixture to ambient temperature
2. 2
   ろ過Filter the resulting mixture
3. 3
   洗浄wash with a large amount of water
4. 4
   その他collect the precipitate

実験手順

Combine 2,4-difluoro-1-nitro-benzene (5.36 g, 33.69 mmol), 2-amino-5-trifluoromethyl-benzonitrile (5.701 g, 30.63 mmol) and lithium hydroxide monohydrate (2.57 g, 61.25 mmol) in methyl sulfoxide (DMSO, 70 ml). Heat the resulting mixture to 55° C. for 16 hours. Cool the reaction mixture to ambient temperature, then pour into approximately 250 ml of ice water and stir for one hour. Filter the resulting mixture, wash with a large amount of water and collect the precipitate to obtain 9.53 g of the title compound (29.30 mmol, 96% yield) as a yellow amorphous solid: Mass Spectrum (m/e): 324(M−1).

出典