Reaction equation
[C:1]([C:5]([C:8]([C:11]([C:14]([C:17]([C:20]([C:23]([CH:26]=[CH2:27])([F:25])[F:24])([F:22])[F:21])([F:19])[F:18])([F:16])[F:15])([F:13])[F:12])([F:10])[F:9])([F:7])[F:6])([F:4])([F:3])[F:2].[Al](I)(I)[I:29].C(=O)=O.CC(C)=O>>[C:1]([C:5]([C:8]([C:11]([C:14]([C:17]([C:20]([C:23]([CH2:26][CH2:27][I:29])([F:24])[F:25])([F:21])[F:22])([F:18])[F:19])([F:16])[F:15])([F:13])[F:12])([F:10])[F:9])([F:7])[F:6])([F:4])([F:3])[F:2]Participants
Conditions
- Temperature
- 130 °C
Procedure
198 g of CF3(CF2)7CH═CH2 and 5 g of AlI3 were charged into a 200-ml stainless-steel autoclave and displacement of the atmosphere with nitrogen was repeated 5 times by vacuum evacuation and charging with nitrogen gas while cooling the autoclave with dry ice/acetone. The oxygen concentration inside the system was not more than 1 ppm and the moisture content was not more than 1 ppm. Thereafter, nitrogen was removed by evacuation and 11 g of hydrogen iodide gas was charged therein. Heating was carried out with stirring for two hours at 130° C. After cooling, the liquid in the autoclave was sampled, and GC analysis (gas chromatography analysis) and GC/MS analysis (gas chromatography/mass analysis) were performed. CF3(CF2)7CH2CH2I was produced at a conversion rate of 2% and at a selectivity of 100%.
Workup
- concentrationThe oxygen concentration inside the system
- customThereafter, nitrogen was removed by evacuation and 11 g of hydrogen iodide gas
- additionwas charged
- temperatureHeating
- temperatureAfter cooling
- aliquotthe liquid in the autoclave was sampled
Sources & evidence
- ORD record
- ord-68debad7f8ee45898bee26df15218051
- Source dataset
- uspto-grants-2005_09
- Patent number
- US06946582B2
Linked notes
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