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

HRID 433033

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HRID 433033 반응식
[Si](=O)=O.[F-:4].[K+].[F:6][C:7]([F:21])([C:11]([F:20])(F)[C:12]([F:18])(F)[C:13]([F:16])([F:15])[F:14])C(O)=O>>[F:4][C:7]([F:6])([F:21])[C:11]([F:20])=[C:12]([F:18])[C:13]([F:14])([F:15])[F:16]

참가 물질

4

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온도
265 °C

실험 절차

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%.

후처리

  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.

출처 및 근거

ORD 기록
ord-2accaab0736a48a1958b5a6c7a0dd82a
출처 데이터셋
uspto-grants-2003_12
특허 번호
US06664431B2

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