Ammonia → HCID 15614241, compound
Reaction equation
F[C:2]1[C:7]([F:8])=[C:6]([F:9])[CH:5]=[C:4]([F:10])[C:3]=1[C:11]([F:14])([F:13])[F:12].[NH3:15]>O1CCCC1>[NH2:15][C:2]1[C:7]([F:8])=[C:6]([F:9])[CH:5]=[C:4]([F:10])[C:3]=1[C:11]([F:14])([F:13])[F:12]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 100 °C
Procedure
110 g of 2,3,4,6-tetrafluoro-benzotrifluoride in 200 ml of tetrahydrofuran were initially introduced into a 0.7 l stainless steel autoclave and it was pressurized using 30 ml of liquid ammonia. The mixture was subsequently heated at 100° C. for 3 hours, a maximum pressure of 10 bar being adjusted. After cooling, the pressure was released and the liquid phase was subjected to a fractional distillation. 42 g of 2-amino-3,4,6-trifluorobenzotrifluoride were first obtained with a boiling point of 47° to 48° C. at 8 mbar, then after an intermediate run, 46 g of 2,5,6-trifluoro-4-amino-benzo-trifluoride with a boiling point of 75° to 78° C. at 8 mbar.
Workup
- temperatureAfter cooling
- distillationthe liquid phase was subjected to a fractional distillation
Sources & evidence
- ORD record
- ord-25a5d19a84184b79810e8184b89a4d32
- Source dataset
- uspto-grants-1992_01
- Patent number
- US05082971
Reaction notes
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