Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium Carbonate → 4-(1-Oxo-indan-5-yloxy)-benzonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 4-Fluorobenzonitrile | HCID 14517 | — |
| 반응물 | 5-Hydroxy-1-indanone | HCID 233147 | — |
| 반응물 | toluene N,N-dimethylacetamide | HCID 66603805 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 4-(1-Oxo-indan-5-yloxy)-benzonitrile | HCID 59750643 | 51.3% |
반응 단계
Combine 5-Hydroxyindanone (2.0 g, 13.50 mmol), 4-Fluorobenzonitrile (1.55 g, 12.80 mmol), K2CO3 (2.65 g, 19.20 mmol) and toluene/DMA (20 ml/40 ml), reflux under Nitrogen using a Dean-Stark Trap. After 4.0 hours, cool the reaction to room temperature and add Ethyl Acetate. Wash several times with 10% LiCl and Brine solution, then dry the organic layer over Na2SO4 follow by concentration. Flash chromatograph using 4/1 then 1/1 hexanes/ethyl acetate eluant to afford 1.64 g, 6.57 mmol (49% yield) of the title compound: 1H NMR (500 MHz, CDCl3); 2.7-2.8 (2H, m), 3.1-3.2 (2H, m), 7.0-7.1 (2H, m), 7.1-7.2 (2H, m), 7.6-7.7 (2H, m), 7.7-7.8 (1H, m); MS m/z 250 (M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07399774B2 |
| 출처 데이터셋 | uspto-grants-2008_07 |
| ORD ID | ord-b6f0d1d89b4a4e5d83b20bef39093f66 |
| 출처 메모 | uspto-grants-2008_07 |