Chlorine → HCID 15014914, compound

Temperature

-10 °C

In a 1000-ml flask equipped with a stirring apparatus and a thermometer were charged 100 ml of m-xylene, 500 ml of a sodium hypochlorite aqueous solution having a 12% available chlorine content and containing 5.0 g of sodium hydroxide, 20.0 g (77.5 mmols) of 3-iodopentafluoropropene and 0.25 g (0.6 mmol) of TOMAC as a catalyst. After the reaction liquid was cooled to -10° C., the reaction liquid was stirred with the stirring apparatus to initiate the reaction. The reaction was continued while maitaining the reaction temperature at -10° C. After the 15 minutes of reaction time lapsed, the conversion of 3-iodopentafluoropropene became almost 100%. Then the reaction liquid was cooled to -30° C. to freeze the aqueous phase, and the organic phase was separated therefrom. After the organic phase was dried over anhydrous sodium sulfate, the product was isolated from the organic phase through fractional distillation twice. Thus, 8.7 g (yield, 41%) of the captioned compound having a boiling point of 52° C. was obtained.

1. customIn a 1000-ml flask equipped with a stirring apparatus
2. customAfter the reaction liquid
3. customthe reaction liquid
4. customthe reaction
5. customat -10° C
6. customAfter the 15 minutes of reaction time
7. customThen the reaction liquid
8. temperaturewas cooled to -30° C.
9. customthe organic phase was separated
10. dry with materialAfter the organic phase was dried over anhydrous sodium sulfate
11. customthe product was isolated from the organic phase through fractional distillation twice
12. customThus, 8.7 g (yield, 41%) of the captioned compound
13. customwas obtained

ORD record

ord-922e4d5bea7440a79caca8ccc823f242

Source dataset

uspto-grants-1991_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05055601