Bromide ion → Perfluorooctyl bromide

HRID 1196178

반응식

HRID 1196178 반응식
[F:1][C:2](I)([F:25])[C:3]([F:24])([F:23])[C:4]([F:22])([F:21])[C:5]([F:20])([F:19])[C:6]([F:18])([F:17])[C:7]([F:16])([F:15])[C:8]([F:14])([F:13])[C:9]([F:12])([F:11])[F:10].[Br-:27]>[Cu](Br)Br>[F:1][C:2]([Br:27])([F:25])[C:3]([F:24])([F:23])[C:4]([F:22])([F:21])[C:5]([F:20])([F:19])[C:6]([F:18])([F:17])[C:7]([F:16])([F:15])[C:8]([F:14])([F:13])[C:9]([F:12])([F:11])[F:10]

참가 물질

4

반응물 2

HCID 259Bromide ionHCID 10491Perfluorooctyl iodide

생성물 1

HCID 9873Perfluorooctyl bromide수율 83.5%

시약·촉매·용매 1

HCID 24611Copper bromide (CuBr2)촉매

실험 절차

13.0 g (0.09 mol) of finely ground copper bromide of the formula CuBr are put into a bomb tube of capacity 25 cm3 and made of glass, and are subjected to a temperature of 200° C. under a pressure of 10 Pa for 4 hours, in order to remove residual water. After the bomb tube has cooled to room temperature, anhydrous nitrogen is passed into it and 16.4 g (0.03 mol) of perfluorooctyl iodide are added, and the bomb tube is sealed by fusion and shaken for 50 hours at 240° to 250° C. 3 mol of bromide ions are employed per mol of bound iodine atom. When the reaction is complete, the bomb tube is opened and the organofluorine products are distilled out of the bomb tube by heating at 200° C. This gives 12.8 g of distillate which, according to analysis by gas chromatography is composed of 97.7% by weight of perfluorooctyl bromide; 1.9% by weight of unreacted perfluorooctyl iodide and 0.3% by weight of CF3 (CF2)7H. This corresponds to a yield of 83.5% of perfluorooctyl bromide, relative to perfluorooctyl iodide employed.

후처리

  1. customto remove residual water
  2. additionare added
  3. customthe bomb tube is sealed by fusion
  4. distillationthe organofluorine products are distilled out of the bomb tube
  5. temperatureby heating at 200° C

출처 및 근거

ORD 기록
ord-f8471c4fcdc0408c955cad3f802ffe96
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05113026

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