関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pentamethyldisiloxane | HCID 74037 | — |
| 反応物 | Benzoic acid, 4-(5-hexenyloxy)-, 4-cyanophenyl ester | HCID 1822389 | — |
| 触媒 | HCID 178479810 | HCID 178479810 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4-Cyanophenyl 4-(6-pentamethyldisiloxanylhexyloxy)benzoate | HCID 19972160 | — |
反応手順
0.94 g (0.024 mmol of Pt) of 0.5% strength dicyclopentadienylplatinum dichloride solution (dichloromethane) was added to a solution of 13.8 g (42.9 mmol) of 4-cyanophenyl 4-(5-hexenyloxy)benzoate and 6.48 g (43.7 mmol) of pentamethyldisiloxane in 50.0 g of toluene, and the mixture was refluxed for 3 hours. After complete hydrosilylation of the olefin, a further 0.94 g (0.024 mmol of Pt) of 0.5% strength dicyclopentadienylplatinum dichloride solution (dichloromethane) were added, and the mixture was refluxed for a further 2 hours. The reaction mixture was flushed with nitrogen, and the toluene was removed by vacuum distillation on a rotary evaporator. The crude product was purified by chromatography on silica gel. The 4-cyanophenyl 4-(6-pentamethyldisiloxanylhexyloxy)benzoate obtained was additionally recrystallized from petroleum ether (100° C.-140° C.) and exhibited the following phase behavior: c 54-55 (sA 53-55) i.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05277838 |
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| 出典データセット | uspto-grants-1994_01 |
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| ORD ID | ord-5723a77c7f4f4bf3a0a6d26b44f3fc07 |
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| 出典メモ | uspto-grants-1994_01 |
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