Fluorotrimethylsilane → 2-Bromo-2-(trifluoromethyl)hexafluoropropane

HRID 1731387

반응식

HRID 1731387 반응식
[Br:1]Br.[F:3][C:4]([F:15])([F:14])[C-:5]([C:10]([F:13])([F:12])[F:11])[C:6]([F:9])([F:8])[F:7].CN([S+](N(C)C)N(C)C)C.FC(F)(F)C(=C(F)F)C(F)(F)F.F[Si](C)(C)C>C(#N)C1C=CC=CC=1>[Br:1][C:5]([C:6]([F:9])([F:8])[F:7])([C:10]([F:11])([F:12])[F:13])[C:4]([F:14])([F:15])[F:3]

참가 물질

6

반응물 4

HCID 9869FluorotrimethylsilaneHCID 24408BromineHCID 611091,1,3,3,3-Pentafluoro-2-(trifluoromethyl)-1-propeneHCID 20228871Tris(dimethylamino)sulfonium 1,1,1,3,3,3-hexafluoro-2-(trifluoromethyl)-2-propanide

생성물 1

HCID 5503852-Bromo-2-(trifluoromethyl)hexafluoropropane수율 81%

시약·촉매·용매 1

HCID 7505Benzonitrile용매

실험 절차

Bromine, 17.25 g (0.108 mol), was added dropwise at 0° to a solution of tris(dimethylamino)sulfonium 1,1,1,3,3,3-hexafluoro-2-(trifluoromethyl)-2-propanide, prepared by dissolving 33.4 g (0.12 mol) of tri(dimethylamino)sulfonium difluorotrimethylsilicate and 24.0 g (0.12 mol) of perfluoroisobutylene in 75 mL of benzonitrile, then pumping out the by-product fluorotrimethylsilane at reduced pressure. The reaction mixture was evacuated to transfer the volatile reaction product into a cold trap (-78°). Sublimation of the contents of the trap at atmospheric pressure gave 26.11 g (81%) of 2-bromo-1,1,1,3,3,3-hexafluoro-2-(trifluoromethyl)propane as a very volatile solid: m.p. (sublimation) 49°-51°; 19F NMR (CDCl3) δ -67.6 ppm (s).

후처리

  1. customprepared
  2. customThe reaction mixture was evacuated
  3. custom(-78°)

출처 및 근거

ORD 기록
ord-8dc7618fcd434ed0a9d5a8bf151fb5e6
출처 데이터셋
uspto-grants-1986_11
특허 번호
US04621126

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