4-Fluoroiodobenzene → HCID 22022614, compound

Temperature

110 °C

26.64 g of p-fluoroiodobenzene, 100 ml of DMSO and 15.24 g of copper powder were put in a flask under an atmosphere of nitrogen to be sufficiently stirred at a temperature of 110° C. Next, 30.46 g of 1,6-diiodoperfluorohexane was slowly dropped and stirred at a temperature of 120° C. for 20 hours. Then, the reaction solution was filtered so as to remove the unreacted copper, and was dropped into an aqueous solution containing a small quantity of NaCl. Then, the resulting deposits were filtered. The deposits were dissolved in acetone to be filtered and thereafter distill out the acetone. The residue was dissolved in methanol to add water and deposits were filtered. The deposits were distilled at a reduced pressure (155° C., 5 mmHg), thereby obtaining 20 g of a colorless solid.

1. stirringstirred at a temperature of 120° C. for 20 hours
2. filtrationThen, the reaction solution was filtered so as
3. customto remove the unreacted copper
4. additionwas dropped into an aqueous solution
5. additioncontaining a small quantity of NaCl
6. filtrationThen, the resulting deposits were filtered
7. dissolutionThe deposits were dissolved in acetone
8. filtrationto be filtered
9. distillationdistill out the acetone
10. dissolutionThe residue was dissolved in methanol
11. additionto add water and deposits
12. filtrationwere filtered
13. distillationThe deposits were distilled at a reduced pressure (155° C., 5 mmHg)

ORD record

ord-62d3050d48154ceb954c41bb923105d6

Source dataset

uspto-grants-2006_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07081497B2