化工社化工社 化学情報印刷レポート · 研究参考用
Picolinic acid → N,N'-Bis(picolinovl)-2.5-diazabicyclo[2 .2.2]octane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Picolinic acid | HCID 1018 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate | HCID 151348 | — |
| 反応物 | 2,5-Diazabicyclo(2.2.2)octane | HCID 423347 | — |
| 反応物 | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | N,N'-Bis(picolinovl)-2.5-diazabicyclo[2 .2.2]octane | HCID 9905241 | — |
反応手順
Combine 2,5-diazabicyclo[2.2.2]octane (1 molar equivalent), picolinic acid (3 molar equivalents), BOP reagent (3 molar equivalents), HOBt hydrate (3 molar equivalents) and iPr2NEt (5 molar eqiuvalents) in DMF. Maintain the reaction at room temperature for 18 h. Quench the reaction by pouring into brine and extracting with EtOAc. Dry the combined organic extracts over Na2SO4 and remove the solvent in vacuo. Purification by flash chromatography gives the title product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06200986B1 |
| 出典データセット | uspto-grants-2001_03 |
| ORD ID | ord-bc07b0f986774c52b74867c3f8109621 |
| 出典メモ | uspto-grants-2001_03 |