関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tributylstannane | HCID 5948 | — |
| 反応物 | Silane, triethoxyethynyl- | HCID 79778 | — |
| 触媒 | Azobisisobutyronitrile | HCID 6547 | — |
| 生成物 | (E)-triethoxy(2-(tributylstannyl)vinyl)silane | HCID 86668310 | 101.4% |
反応手順
Tributyltin hydride (1.9 mL, 7.2 mmol, 1.0 equiv) and triethoxy(ethynyl)silane (1.5 g, 7.9 mmol, 1.1 equiv) were combined. AIBN (60 mg, 0.36 mmol, 0.05 equiv) was added and the resulting yellow solution was heated to 80° C. Upon reaching 80° C., the reaction exothermed to 104° C. The yellow solution was cooled back to 80° C. and stirred for 20 h. The reaction mixture was cooled to provide the title compound as a pale yellow oil (3.5 g, 99% crude yield): IR (thin film) 2957 (s), 2925 (s), 2873 (m), 2854 (m) cm−1; 1H NMR (400 MHz, CDCl3) δ 7.43 (d, J=24 Hz, 1H), 6.37 (d, J=24 Hz, 1H), 3.83 (q, J=7 Hz, 6H), 1.49 (m, 6H), 1.29 (m, 6H), 1.22 (t, J=7 Hz, 9 H), 0.82-0.92 (m, 15 H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08658568B2 |
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| 出典データセット | uspto-grants-2014_02 |
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| ORD ID | ord-48b6901412864ccaa3a78bc1e1853cf1 |
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| 出典メモ | uspto-grants-2014_02 |
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