関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Trimethyl borate | HCID 8470 | — |
| 反応物 | 1,3-Dimethoxybenzene | HCID 9025 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (2,6-Dimethoxyphenyl)boronic acid | HCID 2734343 | — |
反応手順
1,3-Dimethoxybenzene (4 g) was dissolved in freshly distilled THF (10 mL). This solution was cooled to −78° C. and n-BuLi (24 mL, 1.6 M solution in hexanes) was added dropwise to the cold solution. The mixture was stirred at −78° C. for 1 h, then warmed to room temperature and stirred for 1 h. The resulting mixture was cooled again to −78° C. and (MeO)3B (6.7 mL) was added. The mixture was allowed to warm to room temperature and stirred overnight. Water (10 mL) was added, and the mixture was stirred for 0.5 h, acidified to pH 4 with acetic acid and extracted with EtOAc. The extract was dried (MgSO4) and evaporated to give 2,6-dimethoxybenzeneboronic acid, which was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06855843B2 |
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| 出典データセット | uspto-grants-2005_02 |
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| ORD ID | ord-d59ade9a59d241b4931c9e0bd6130bdd |
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| 出典メモ | uspto-grants-2005_02 |
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