Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Picolinic acid → N,N'-Bis(picolinovl)-2.5-diazabicyclo[2 .2.2]octane
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Picolinic acid | HCID 1018 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate | HCID 151348 | — |
| 반응물 | 2,5-Diazabicyclo(2.2.2)octane | HCID 423347 | — |
| 반응물 | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Sodium chloride; water | HCID 57417360 | — |
| 생성물 | N,N'-Bis(picolinovl)-2.5-diazabicyclo[2 .2.2]octane | HCID 9905241 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06200986B1 |
| 출처 데이터셋 | uspto-grants-2001_03 |
| ORD ID | ord-bc07b0f986774c52b74867c3f8109621 |
| 출처 메모 | uspto-grants-2001_03 |