関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chlorotrimethylsilane | HCID 6397 | — |
| 反応物 | 1,2-Dibromoethane | HCID 7839 | — |
| 反応物 | Zinc | HCID 23994 | — |
| 反応物 | Dichlorobenzyl chloride | HCID 76790 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 178478089 | HCID 178478089 | — |
反応手順
Under an argon stream, to a suspension of zinc powder (55.1 g, 843 mmol) in tetrahydrofuran (THF; 56 ml) was added 1,2-dibromoethane (2.9 ml, 33.8 mmol) and the mixture was heated under reflux for 5 min. Then, trimethylsilyl chloride (8.6 ml, 67.5 mmol) was added at 0° C. and the mixture was stirred at 0° C. for 5 min, after which a solution of 2,3-dichlorobenzyl chloride (82.4 g, 421.7 mmol) in THF (330 ml) was added dropwise with ice-cooling. After completion of the dropwise addition, the mixture was warmed to room temperature and stirred for 1 hr to give a solution of 2,3-dichlorobenzylzinc chloride in THF.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07176220B2 |
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| 出典データセット | uspto-grants-2007_02 |
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| ORD ID | ord-6c552893a17c45cd95cacf07d34e3298 |
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| 出典メモ | uspto-grants-2007_02 |
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