Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 2,5-Dichloro-pyridine-3-carbaldehyde
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Tributylstannane | HCID 5948 | — |
| 반응물 | 2,5-Dichloro-nicotinoyl chloride | HCID 2799996 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2,5-Dichloro-pyridine-3-carbaldehyde | HCID 21973274 | 34.4% |
반응 단계
To a solution of 2,5-Dichloro-nicotinoyl chloride (15 g, 0.071 mol) in tetrahydrofuran was added tributyl-stannane (24.9 g, 0.086 mol) portionwise over 45 minutes. The resulting mixture was stirred at ambient temperature for 50 minutes, and then treated with tetrakis(triphenylphosphine)palladium(0) (0.82 g, 0.00071 mol). The reaction mixture was stirred at ambient temperature for 4 hours, poured into water; the product was extracted with ethylacetate, the combined organics were dried over magnesium sulfate, filtered and concentrated in vacuo. Silica gel chromatography (10% ethyl acetate/hexanes) followed by recrystallization from hexanes/ethylacetate gave the title compound (4.3 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07098212B2 |
| 출처 데이터셋 | uspto-grants-2006_08 |
| ORD ID | ord-38c6d934eb854ee7a469257bfdad0650 |
| 출처 메모 | uspto-grants-2006_08 |