関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dichlorodimethylsilane | HCID 6398 | — |
| 反応物 | 1,2-Dichloro-1,1,2,2-tetramethyldisilane | HCID 78045 | — |
| 反応物 | 4-Cyanobenzoyl chloride | HCID 80172 | — |
| 反応物 | HCID 178418416 | HCID 178418416 | — |
| 触媒 | Triphenylphosphine | HCID 11776 | — |
| 触媒 | Bis(benzonitrile)palladium chloride | HCID 498840 | — |
| 生成物 | 4-Chlorodimethylsilylbenzonitrile | HCID 131715395 | 60% |
反応手順
A reaction mixture containing 10 gm (6×10-2 mole) of p-cyanobenzoyl chloride and 15 gm (1.25 mole equivalent) of 1,2-dichlorotetramethyldisilane was heated to 135° C. during which time the solution became homogeneous. A cocatalyst mixture containing 200 mg. bis(benzonitrile)palladiumdichloride (1 mole %) and 274 mg triphenylphosphine (2 mole %) was then introduced. Carbon monoxide gas evolution began immediately and the reaction was heated at 140° C. for 12 hours while dimethyldichlorosilane was continuously removed. Vacuum distillation gave 7 gm (60% isolated yield) of 4-chlorodimethylsilylbenzonitrile, bp. 93°/0.1 torr, m.p. 40°-43° C. The resulting chlorodimethylsilylbenzonitrile, in the form of a low melting high moisture sensitive solid was hydrolyzed to the corresponding 1,3-bis(4'-benzonitrile)tetramethyldisiloxane in the form of a colorless liquid. The identity of the disiloxane was further confirmed by its NMR and IR spectra.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04709054 |
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| 出典データセット | uspto-grants-1987_11 |
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| ORD ID | ord-cb6a7eabdcee432a8f29787889f303d6 |
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| 出典メモ | uspto-grants-1987_11 |
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