Tetraethoxysilane → Bis(pentafluorophenyl)diethoxysilane

HRID 11977

반응식

HRID 11977 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 mol, 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-a93a27bfb7fd4c638aa74d18829c69e1
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07098346B2

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