Chlorotrifluoroethylene → 4-Chloro-3-methyl-4,5,5-trifluorocyclohexene
Reaction equation
[Cl:1][C:2]([F:6])=[C:3]([F:5])[F:4].[CH2:7]=[CH:8][CH:9]=[CH:10][CH3:11]>>[Cl:1][C:2]1([F:6])[C:3]([F:5])([F:4])[CH2:7][CH:8]=[CH:9][CH:10]1[CH3:11]Participants
3
Procedure
A flow reactor equipped with dual tubes having 20 mm of inner diameter of the outer tube, 16 mm of outer diameter of the inner tube, and 60 cm of length of the tubes was employed. The temperature in the reactor was kept at 520° C. Chlorotrifluoroethylene (CTFE), 1,3-pentadiene and nitrogen gas were continuously injected into the flow reactor at the rates of 36.1 g/hr, 20.4 g/hr, and 0.4 mol/hr, respectively, and the vapor phase condensation was carried out for 1 hour. Then, 4.7 g of unreacted chlorotrifluoroethylene (CTFE) was recovered. The resultant was purified by steam distillation, and then the water layer was removed to give 32.1 g of the mixture (GC%=52%).
Workup
- customA flow reactor equipped with dual tubes
- customwas kept at 520° C
- customrespectively, and the vapor phase condensation
- customThen, 4.7 g of unreacted chlorotrifluoroethylene (CTFE) was recovered
- distillationThe resultant was purified by steam distillation
- customthe water layer was removed
Sources & evidence
- ORD record
- ord-56e97af30ff44b729c8c1d17932aef13
- Source dataset
- uspto-grants-1999_12
- Patent number
- US06008407
Reaction notes
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