Aluminum iodide → Decane, 1,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8-heptadecafluoro-10-iodo-

HRID 496955

반응식

HRID 496955 반응식
[C:1]([C:5]([C:8]([C:11]([C:14]([C:17]([C:20]([C:23]([CH:26]=[CH2:27])([F:25])[F:24])([F:22])[F:21])([F:19])[F:18])([F:16])[F:15])([F:13])[F:12])([F:10])[F:9])([F:7])[F:6])([F:4])([F:3])[F:2].[Al](I)(I)[I:29].C(=O)=O.CC(C)=O>>[C:1]([C:5]([C:8]([C:11]([C:14]([C:17]([C:20]([C:23]([CH2:26][CH2:27][I:29])([F:24])[F:25])([F:21])[F:22])([F:18])[F:19])([F:16])[F:15])([F:13])[F:12])([F:10])[F:9])([F:7])[F:6])([F:4])([F:3])[F:2]

참가 물질

4

반응물 3

HCID 82222Aluminum iodideHCID 889901H,1H,2H-Perfluoro-1-deceneHCID 18522661Acetone cardice

생성물 1

HCID 74885Decane, 1,1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8-heptadecafluoro-10-iodo-

반응 조건

온도
130 °C

실험 절차

198 g of CF3(CF2)7CH═CH2 and 5 g of AlI3 were charged into a 200-ml stainless-steel autoclave and displacement of the atmosphere with nitrogen was repeated 5 times by vacuum evacuation and charging with nitrogen gas while cooling the autoclave with dry ice/acetone. The oxygen concentration inside the system was not more than 1 ppm and the moisture content was not more than 1 ppm. Thereafter, nitrogen was removed by evacuation and 11 g of hydrogen iodide gas was charged therein. Heating was carried out with stirring for two hours at 130° C. After cooling, the liquid in the autoclave was sampled, and GC analysis (gas chromatography analysis) and GC/MS analysis (gas chromatography/mass analysis) were performed. CF3(CF2)7CH2CH2I was produced at a conversion rate of 2% and at a selectivity of 100%.

후처리

  1. concentrationThe oxygen concentration inside the system
  2. customThereafter, nitrogen was removed by evacuation and 11 g of hydrogen iodide gas
  3. additionwas charged
  4. temperatureHeating
  5. temperatureAfter cooling
  6. aliquotthe liquid in the autoclave was sampled

출처 및 근거

ORD 기록
ord-68debad7f8ee45898bee26df15218051
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06946582B2

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