関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Dodecene | HCID 8183 | — |
| 反応物 | Dichlorosilane | HCID 61330 | — |
| 触媒 | Platinate(2-), hexachloro-, hydrogen, hydrate (1:2:1), (OC-6-11)- | HCID 16211507 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | Dichlorodidodecylsilane | HCID 21889369 | — |
反応手順
To a dry tarred 500 mL Schlenk bomb flask was condensed 29.0 g (0.286 mol) of dichlorosilane at −78° C. To this was added 100 g (0.594 mol) of 1-dodecene under an argon flow. This mixture was allowed to warm to 0° C., then 100 mg (0.193 mmol) of hexachloroplatinic acid hexahydrate dissolved in 2 mL of isopropanol was added via syringe. The mixture was allowed to slowly warm to room temperature where it was allowed to stir for 40 hours. After this time the solution was cannula transferred into a dry 250 mL 3-necked round bottom flask equipped with a fractional distillation apparatus. The mixture was distilled at 220° C. at 0.1 mmHg. Yield: 78.1 g (62.5%). 1H NMR (400 MHz, C6D6): δ=1.6-1.4 (m, 4H), 1.4-1.1 (m, 36H), 1.0-0.8 (m, 10H). 13C NMR (100 MHz, C6D6): δ=33.19, 32.72, 30.51, 30.30, 30.21, 29.89, 23.51, 23.16, 20.92, 14.77. HRMS (EI) m/z, calcd for C24H50Cl2Si (M+): 436.3059; found: 436.3058.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08343382B2 |
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| 出典データセット | uspto-grants-2013_01 |
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| ORD ID | ord-a479cd8cd4bf40a4823c0309ae2e79a7 |
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| 出典メモ | uspto-grants-2013_01 |
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