Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Iodine → HCID 178451733, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Iodine | HCID 807 | — |
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | Sodium Thiosulfate | HCID 24477 | — |
| 반응물 | 4-(1H-indazol-6-yl)-3,6-dihydro-2H-pyridine-1-carboxylic acid tert-butyl ester | HCID 67449416 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 178451733 | HCID 178451733 | — |
반응 단계
A solution of 4-(1H-indazol-6-yl)-3,6-dihydro-2H-pyridine-1-carboxylic acid tert-butyl ester (9.70 g, 3.24 mmol) in DMF (32 mL) at room temperature was treated with iodine (1.23 g, 4.86 mmol) and KOH (grounded, 454 mg, 8.1 mmol). The resulting mixture was stirred at room temperature for 40 min, then treated with saturated Na2S2O3 aqueous solution. The resulting mixture was then extracted with EtOAc (3×). The combined extracts were washed with brine and dried over Na2SO4. The resulting mixture was filtered and concentration under reduced pressure. The resulting residue was purified by flash chromatography on silica-gel (gradient eluant 10% to 40% EtOAc in heptane) to yield the title compound as white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08822447B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-98c16b4a4f534f93ada601a2380dd571 |
| 출처 메모 | uspto-grants-2014_09 |