Silica → 1,1,1,2,3,4,4,4-Octafluorobut-2-ene

Temperature

265 °C

A 0.3 dm3-capacity tubular reactor made from stainless steel, provided with electric heating, with a thermocouple sheath, with pipes for feeding the starting components and discharging the reaction products, is charged with about 0.23 dm3 of a catalyst which is silicon dioxide promoted with potassium fluoride in an amount of 35 wt. %. The catalyst is heated in a stream of dry nitrogen with a gradual temperature increase from 180 to 350° C. for four hours. Then the temperature is lowered to 240° C., and 40 g of methyl ester of perfluorovaleric acid are fed with the rate of 20 g/hour. The gas mixture outgoing from the reactor is condensed in a trap cooled down to −30° C., and subjected to low-temperature rectification, as a result of which 27.4 g of perfluoro-2-butene are obtained. The yield of the target product is 95.1%.

1. customprovided with electric heating, with a thermocouple sheath, with pipes
2. temperatureThe catalyst is heated in a stream of dry nitrogen with a gradual temperature
3. customis lowered to 240° C.
4. customcondensed in a trap
5. temperaturecooled down to −30° C.

ORD record

ord-2accaab0736a48a1958b5a6c7a0dd82a

Source dataset

uspto-grants-2003_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06664431B2