Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium Carbonate → 1-Ethynyl-2-fluoro-3-methoxybenzene
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2-Fluoro-3-methoxybenzaldehyde | HCID 3774463 | — |
| 반응물 | Dimethyl-1-diazo-2-oxopropylphosphonate | HCID 86586111 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 1-Ethynyl-2-fluoro-3-methoxybenzene | HCID 82810771 | 92.2% |
반응 단계
Potassium carbonate (3.6 g, 26.0 mmol) and dimethyl-1-diazo-2-oxopropylphosphonate (2.4 mL, 15.6 mmol) were added sequentially to a solution of 2-fluoro-3-methoxybenzaldehyde (2.0 g, 13.0 mmol) in methanol (100 mL), and the reaction was allowed to stir at room temperature for 16 h. After concentrating the reaction mixture under reduced pressure, the crude material was purified by flash chromatography (40 g silica gel column, 0-40% gradient ethyl acetate in hexanes) to provide a clear colorless oil (1.8 g, 92%). MS (GCMS) m/z 150. 1H NMR (400 MHz, CHLOROFORM-d) δ3.31 (d, J=0.78 Hz, 1H) 3.90 (s, 3H) 6.93-7.11 (m, 3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08748466B2 |
| 출처 데이터셋 | uspto-grants-2014_06 |
| ORD ID | ord-0ee9c85b54f14a6d9bf2444ee02b6e73 |
| 출처 메모 | uspto-grants-2014_06 |