Tetraethoxysilane → Trifluorovinyl triethoxysilane

HRID 11976

反応式

HRID 11976 の反応式
[C:1](=[C:4](Cl)[F:5])([F:3])[F:2].[Li]C(CC)C.[Si:12](OCC)([O:19][CH2:20][CH3:21])([O:16][CH2:17][CH3:18])[O:13][CH2:14][CH3:15]>CCOCC>[C:1](=[C:4]([Si:12]([O:19][CH2:20][CH3:21])([O:16][CH2:17][CH3:18])[O:13][CH2:14][CH3:15])[F:5])([F:3])[F:2]

参加物

5

反応物 3

HCID 6517TetraethoxysilaneHCID 6594ChlorotrifluoroethyleneHCID 178418400CID 53628100

生成物 1

HCID 21864279Trifluorovinyl triethoxysilane

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
-80 °C

実験手順

200 ml of freshly distilled dry Et2O is added to a 500 ml vessel (under an argon atmosphere). The vessel is cooled down to −80° C. and 15 g (0.129 mol) of CF2═CFCl gas is bubbled to Et2O. 100 ml (0.13 mol) of sec-BuLi is added dropwise during three hours. The temperature of the solution is kept below −60° C. all the time. The solution is stirred for 15 minutes and 29 ml (27.08 g, 0.130 mol) of Si(OEt)4 is added in small portions. The solution is stirred for over night allowing it to warm up to room temperature. Formed red solution is filtered and evaporated to dryness to result crude trifluorovinyltriethoxysilane, CF2═CFSi(OEt)3.

後処理

  1. distillation200 ml of freshly distilled dry Et2O
  2. additionis added to a 500 ml vessel (under an argon atmosphere)
  3. customis kept below −60° C.
  4. stirringThe solution is stirred for over night
  5. temperatureto warm up to room temperature
  6. customFormed red solution
  7. filtrationis filtered
  8. customevaporated to dryness

出典と根拠

ORDレコード
ord-5458c1810da14b22b17018798e405eb9
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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