Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
5-iodo-N-methoxy-N-methyl-1H-indazole-3-carboxamide → 5-formyl-N-methoxy-N-methyl-1H-indazole-3-carboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 5-iodo-N-methoxy-N-methyl-1H-indazole-3-carboxamide | HCID 20580738 | — |
| 반응물 | HCID 178526064 | HCID 178526064 | — |
| 촉매 | HCID 178418476 | HCID 178418476 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Sodium chloride; water | HCID 57417360 | — |
| 생성물 | 5-formyl-N-methoxy-N-methyl-1H-indazole-3-carboxamide | HCID 24958743 | 15.6% |
반응 단계
A mixture of 5-iodo-N-methoxy-N-methyl-1H-indazole-3-carboxamide (5 g, 15.1 mmol), HCOONa (1.85 g, 30.2 mmol), and PdCl2(PPh3)2 (320 mg, 0.453 mmol) in DMF (20 mL) was put under vacuum, and charged with CO. This process was repeated three times, and the mixture was kept at 110° C. for 6 hr. After cooling to rt, the reaction mixture was diluted with brine and extracted with EtOAc. The organic phases were combined, washed with brine, dried, and concentrated. The crude product was purified by column chromatography to afford 5-formyl-N-methoxy-N-methyl-1H-indazole-3-carboxamide (550 mg, 15.6%) as a white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08198456B2 |
| 출처 데이터셋 | uspto-grants-2012_06 |
| ORD ID | ord-0b44a3f09b694ce1b9e28c3b5e4698c1 |
| 출처 메모 | uspto-grants-2012_06 |