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 | Isophthalonitrile | HCID 12276 | — |
| 反応物 | Lithium diisopropylamide | HCID 2724682 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (2,6-Dicyanophenyl)boronic acid | HCID 22571817 | — |
反応手順
1,3-Dicyanobenzene (1.00 g) was dissolved in freshly distilled THF (70 mL). This solution was cooled to −96° C. and LDA (4.2 mL of a 2M solution) was added dropwise to the cold solution under N2. The mixture was stirred for 30 min at −96° C. and (MeO)3B (1.3 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. The residue was taken up in CH2Cl2, filtered and evaporated to yield 2,6-dicyanobenzeneboronic acid (0.56 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-ee26bd4b04f6458fba5b11f5bfdac889 |
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| 出典メモ | uspto-grants-2005_02 |
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