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>[NH2:14][C:4]1[CH:5]=[C:6]([F:8])[CH:7]=[C:2]([F:1])[C:3]=1[C:10]([F:13])([F:12])[F:11]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 120 °C
Procedure
In a stainless steel autoclave, 200 ml of tetrahydrofuran and 50 g of 2,4,6-trifluorobenzotrifluoride are introduced, and 30 ml of liquid ammonia are pressed on. The mixture is then heated at 120° C. for 6 hours, with stirring. The reaction mixture is cooled, the pressure is released, and the mixture is subjected to fractional distillation. At a boiling point of 57° to 58° C. at 12 mbar, 15 g of 2-amino-4,6-difluoro-benzotrifluoride are obtained. After a small intermediate cut, 32 g of 2,6-difluoro-4-amino-benzotrifluoride distil over at a boiling point of 103° to 105° C. at 16 mbar. Melting point of the resultant 2,6-difluoro-4-amino-benzotrifluoride: 66° C.
Workup
- temperatureThe reaction mixture is cooled
- distillationthe mixture is subjected to fractional distillation
Sources & evidence
- ORD record
- ord-43ddf55f690142f189a5584047384029
- Source dataset
- uspto-grants-1990_08
- Patent number
- US04952601
Reaction notes
Loading…