関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methane | HCID 297 | — |
| 反応物 | 1,1,3,3-Tetramethyl-disiloxane | HCID 18659 | — |
| 反応物 | N-Allylaniline | HCID 68525 | — |
| 触媒 | Chloroplatinic acid | HCID 61859 | — |
| 生成物 | 1,3-bis(N-phenyl-3-aminopropyl)-1,1,3,3-tetramethyldisiloxane | HCID 19871403 | — |
反応手順
N-allylaniline (0.200 mole) and 1,1,3,3-tetramethyldisiloxane (0.100 mole) are introduced along with 0.05 g hexachloroplatinic acid into a 100 ml cylindrical glass reactor equipped with reflux condenser, nitrogen inlet, and stir bar. The contents of the reaction are heated and maintained while stirring, at approximately 70° C., for a period of ten hours. The IR spectrum of the resulting viscous oil shows no peaks corresponding to Si-H, indicating completion of the reaction. The crude product is mixed with carbon black and stirred overnight at room temperature. The product is filtered through silica gel and the filter cake washed with toluene. Volatile fractions are removed by stripping under vacuum at 150° C. to give a slightly colored oil. The oil is further purified by vacuum distillation at <1 torr at 223°-230° C. The yield of 1,3-bis(N-phenyl-3-aminopropyl)-1,1,3,3-tetramethyldisiloxane is virtually quantitative.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04892918 |
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| 出典データセット | uspto-grants-1990_01 |
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| ORD ID | ord-b3c1c43cea734e349539c588f022c8af |
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| 出典メモ | uspto-grants-1990_01 |
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