Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
sodium thiosulfite anhydrous → 6-[(5-Fluoro-2-methoxy-pyridin-3-ylmethyl)-amino]-pyridine-3-carbaldehyde
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | sodium thiosulfite anhydrous | HCID 15847209 | — |
| 반응물 | {6-[(5-Fluoro-2-methoxy-pyridin-3-ylmethyl)-amino]pyridin-3-yl}-methanol | HCID 58259120 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 6-[(5-Fluoro-2-methoxy-pyridin-3-ylmethyl)-amino]-pyridine-3-carbaldehyde | HCID 86653326 | — |
반응 단계
To {6-[(5-fluoro-2-methoxy-pyridin-3-ylmethyl)-amino]-pyridin-3-yl}-methanol (92, 0.353 g, 1.34 mmol) dissolved in 8 mL of tetrahydrofuran, Dess-Maritn periodinane (0.626 g, 1.47 mmol) was added and the reaction stirred at room temperature for 1 hour. The reaction was poured into aqueous saturated sodium thiosulfite and the aqueous layer was extracted with ethyl acetate. The combined organic layer was washed with brine, dried over sodium sulfate, filtered and the filtrate concentrated under vacuum. The resulting material was purified by silica gel column chromatography eluting with ethyl acetate and hexane. Appropriate fractions were combined and concentrated under vacuum to provide the desired compound. MS (ESI) [M+H+]+=262.3.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09096593B2 |
| 출처 데이터셋 | uspto-grants-2015_08 |
| ORD ID | ord-510c1f871672421eba91ddc709628ff1 |
| 출처 메모 | uspto-grants-2015_08 |