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1,1',1''-(Chlorosilylidyne)tris(benzene) → Azidotriphenylsilane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,1',1''-(Chlorosilylidyne)tris(benzene) | HCID 6458 | — |
| 反応物 | Lithium azide | HCID 88163 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Azidotriphenylsilane | HCID 79708 | 86.3% |
反応手順
Following the method of Wiberg et al [Wiberg et al, Angew. Chem. Internat'l Ed.Engl., 1, 335 (1962)] in an inert atmosphere enclosure a solution of triphenylsilylchloride (73.9 g, 0.251 mol) in tetrahydrofuran (400 ml) was stirred with lithium azide (15.3 g, 0.312 mol) at room temperature over a period of 115 hr. After filtration, the solvent was removed in vacuo. The resulting white solid was boiled with heptane (350 ml), filtered hot and allowed to crystallize. Triphenylsilyl azide, 65.5 g (86.3% yield), mp 82°-84° C. was obtained. The melting point and infrared spectrum were identical with that of an authentic sample.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04200721 |
| 出典データセット | uspto-grants-1980_04 |
| ORD ID | ord-57317efd2eb0474482bf61eba626dfaf |
| 出典メモ | uspto-grants-1980_04 |