Tetraethoxysilane → Bis(pentafluorophenyl)diethoxysilane

HRID 584331

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HRID 584331 반응식
Br[C:2]1[C:7]([F:8])=[C:6]([F:9])[C:5]([F:10])=[C:4]([F:11])[C:3]=1[F:12].[Mg].C(O[Si:17]([O:24][CH2:25][CH3:26])([O:21][CH2:22][CH3:23])OCC)C>CCOCC>[F:8][C:7]1[C:2]([Si:17]([C:2]2[C:3]([F:12])=[C:4]([F:11])[C:5]([F:10])=[C:6]([F:9])[C:7]=2[F:8])([O:21][CH2:22][CH3:23])[O:24][CH2:25][CH3:26])=[C:3]([F:12])[C:4]([F:11])=[C:5]([F:10])[C:6]=1[F:9]

참가 물질

5

반응물 3

HCID 6517TetraethoxysilaneHCID 9578BromopentafluorobenzeneHCID 5462224Magnesium

생성물 1

HCID 11102434Bis(pentafluorophenyl)diethoxysilane

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

반응 조건

온도
35 °C

실험 절차

265.2 mL (1.95 mol, 525.353 g) bromopentafluorobenzene, 52.11 g (2.144 mol) magnesium powder and 216 mL (0.975 molt 203.025 g) tetraethoxysilane are mixed together at room temperature and diethylether is added dropwise to the vigorously stirred solution until an exothermic reaction is observed (˜240 mL). The solution is stirred for 30 minutes after which additional 90 mL of Et2O is carefully added. After stirring at 35° C. for 16 h the mixture is cooled to room temperature and diethylether evaporated. An excess of n-heptane (˜600 mL) is added to precipitate the magnesium salts. Solution is filtrated and evaporated to dryness. The residue is fractionally distilled under reduced pressure to yield di(pentafluorophenyl)diethoxysilane.

후처리

  1. additionis carefully added
  2. temperatureis cooled to room temperature
  3. customdiethylether evaporated
  4. additionAn excess of n-heptane (˜600 mL) is added
  5. customto precipitate the magnesium salts
  6. filtrationSolution is filtrated
  7. customevaporated to dryness
  8. distillationThe residue is fractionally distilled under reduced pressure

출처 및 근거

ORD 기록
ord-b49099e9420944be910de1a7a6310513
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06924384B2

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