Chloropentafluorobenzene → Bis(pentafluorophenyl)diethoxysilane

HRID 1180459

反応式

HRID 1180459 の反応式
Cl[C:2]1[C:7]([F:8])=[C:6]([F:9])[C:5]([F:10])=[C:4]([F:11])[C:3]=1[F:12].[Li]C(CC)C.[CH2:18]([O:20][Si:21]([O:34][CH2:35][CH3:36])(Cl)[C:22]1[C:27]([F:28])=[C:26]([F:29])[C:25]([F:30])=[C:24]([F:31])[C:23]=1[F:32])[CH3:19]>CCOCC>[F:8][C:7]1[C:2]([Si:21]([C:22]2[C:23]([F:32])=[C:24]([F:31])[C:25]([F:30])=[C:26]([F:29])[C:27]=2[F:28])([O:34][CH2:35][CH3:36])[O:20][CH2:18][CH3:19])=[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 9579ChloropentafluorobenzeneHCID 21864267DiethoxychloropentafluorophenylsilaneHCID 178418400CID 53628100

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
-70 °C

実験手順

39.52 g (0.195 mol) chloropentafluorobenzene is weighed to a 1000 mL vessel and 250 mL Et2O is added. The vessel is cooled down to −70° C. and 150 mL (0.195 mol) of sec-BuLi (1.3 M) is added dropwise during one hour. The temperature of the solution is kept below −50° C. all the time. The solution is stirred for 30 minutes and 62.54 g (0.195 mol) of diethoxychloropentafluorophenylsilane in Et2O (100 mL) is added in small portions. The solution is stirred for over night allowing it to warm up to room temperature. Formed clear solution is filtered and evaporated to dryness to result di(pentafluorophenyl)diethoxysilane, (C6F5)2Si(OEt)2.

後処理

  1. customis kept below −50° C.
  2. stirringThe solution is stirred for over night
  3. temperatureto warm up to room temperature
  4. customFormed clear solution
  5. filtrationis filtered
  6. customevaporated to dryness

出典と根拠

ORDレコード
ord-44f9eab965c44132bee0ac6d3385b1c3
出典データセット
uspto-grants-2007_10
特許番号
US07280731B2

関連ノート

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