Tetraethoxysilane → Bis(pentafluorophenyl)diethoxysilane

HRID 11977

反応式

HRID 11977 の反応式
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]

参加物

5

反応物 3

HCID 6517TetraethoxysilaneHCID 9578BromopentafluorobenzeneHCID 5462224Magnesium

生成物 1

HCID 11102434Bis(pentafluorophenyl)diethoxysilane

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

反応条件

温度
35 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a93a27bfb7fd4c638aa74d18829c69e1
出典データセット
uspto-grants-2006_08
特許番号
US07098346B2

関連ノート

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