Ammonia → 3,5-Difluoro-2-(trifluoromethyl)aniline
Reaction equation
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[C:4](F)[C:3]=1[C:10]([F:13])([F:12])[F:11].[NH3:14]>O1CCCC1>[F:11][C:10]([F:13])([F:12])[C:3]1[C:2]([F:1])=[CH:7][C:6]([F:8])=[CH:5][C:4]=1[NH2:14]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 120 °C
Procedure
200 ml of tetrahydrofuran and 50 g of 2,4,6-tri-fluorobenzotrifluoride are initially introduced into a stainless steel autoclave, and 30 ml of liquid ammonia are injected. The batch is then heated to 120° C. for 6 hours and with stirring. The reaction mixture is cooled,the pressure is released and the reaction mixture subjected to fractional distillation. At a boiling point of 57° C.-58° C./12 mbar, 15 g of 2-trifluoromethyI-3,5-difluoroaniline are obtained. After a small intermediate fraction 32 g of 3,5-difluoro-4-trifluoromethylaniline distil over at a boiling point of 103° C.-105° C./16 mbar (melting point: 66° C.).
Workup
- distillationthe reaction mixture subjected to fractional distillation
Sources & evidence
- ORD record
- ord-2bb3152e279748e792f36cd2a06703bf
- Source dataset
- uspto-grants-1992_03
- Patent number
- US05096928
Reaction notes
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