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-Bromo-2,6-dichlorobenzene | HCID 29568 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 2,6-Dichlorobenzeneboronic acid | HCID 2734332 | — |
反応手順
1-Bromo-2,6-dichlorobenzene (2.00 g) was dissolved in freshly distilled THF (7 mL). This solution was cooled to −78° C. and n-BuLi (8.3 mL of a 1.6M solution in hexane) was added dropwise to the cold solution under N2. The mixture was stirred for 5 min at −78° C. and (MeO)3B (2.2 mL) was added. The resulting mixture was allowed to warm to room temperature and stirred overnight. Water was added and the resulting mixture was stirred for 0.5 h, then acidified with HOAc and extracted with EtOAc. The organic layer was further washed with water and brine, dried (MgSO4) filtered and evaporated to yield 2,6-dichlorobenzeneboronic acid (1.6 g).
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-4c5b70b56b314212ba05587c2efe66d4 |
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| 出典メモ | uspto-grants-2005_02 |
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