関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | 4-Vinyl-1-cyclohexene | HCID 7499 | — |
| 反応物 | 1,1,3,3-Tetramethyl-disiloxane | HCID 18659 | — |
| 反応物 | (2-Cyclohexenyl)ethyl-1,1,3,3-tetramethyldisiloxane | HCID 131717887 | — |
| 溶媒 | 2-Methyl-2-butanol | HCID 6405 | — |
| 溶媒 | Methyl Ethyl Ketone | HCID 6569 | — |
| 生成物 | HCID 19766624 | HCID 19766624 | — |
反応手順
To a 20 ml toluene solution of 51.93 g (0.48 mole) of 4-vinylcyclohexene-1 and 0.37 g of 5% H2PtCl6 in t-amyl alcohol is added 33.6 (0.23 mole, 90% purity) of 1,1,3,3-tetramethyldisiloxane at 45° C. to 50° C. for 1 hour and 30 minutes. The reaction is complete after maintaining the reaction at 55° C. for 5 hours. To this mixture is added 250 ml methyl ethyl ketone. After washing successively with four 100 ml portions of H2O, 78 g (>95% purity by GC) of 1,3-bis-((2-cyclohexenyl)-ethyl)-1,1,3,3-tetramethyldisiloxane having a light yellowish color is obtained after stripping off solvent at 120° C. and <10 mm Hg. The structure of the product, 1,3-bis-((2-cyclohexenyl)ethyl-1,1,3,3-tetramethyldisiloxane, is confirmed by IR and 1H NMR as follows:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05206312 |
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| 出典データセット | uspto-grants-1993_04 |
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| ORD ID | ord-a6d8ebebae13474784af189af822e12d |
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| 出典メモ | uspto-grants-1993_04 |
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