関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chlorotrimethylsilane | HCID 6397 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 1-Bromo-3-ethynylbenzene | HCID 11480818 | — |
| 反応物 | HCID 86605439 | HCID 86605439 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | ((3-Bromophenyl)ethynyl)trimethylsilane | HCID 3683324 | — |
反応手順
Under an inert atmosphere, 9.5 g of the compound of Step A were introduced into 100 g of tetrahydrofuran, and at 25° C.±3° C., over 15 minutes, 69 ml of a 0.8M solution of magnesium ethyl bromide were added, with stirring for 15 minutes at 25° C. Then, over 2 minutes and without cooling, 8 ml of trimethylsilyl chloride were added with stirring for 30 minutes at 25° C. The reaction mixture was poured into a 2M aqueous solution of NH4Cl and was extracted with ether, dried, filtered, and the filtrate was concentrated to dryness by distilling under reduced pressure then rectified to obtain 12.1 g of 3-(trimethylsilylethynyl)bromobenzene with a boiling point at 0.05 mm/Hg=78° to 84° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04912097 |
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| 出典データセット | uspto-grants-1990_03 |
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| ORD ID | ord-b45ad6403f1a42f39b80f269ce0cdad9 |
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| 出典メモ | uspto-grants-1990_03 |
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