Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 1-(4-Fluorophenyl)-4-oxocyclohexanecarbonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Methyl 5-cyano-5-(4-fluorophenyl)-2-oxocyclohexanecarboxylate | HCID 12230235 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 1-(4-Fluorophenyl)-4-oxocyclohexanecarbonitrile | HCID 91805 | 62.9% |
반응 단계
101.5 g of 5-Cyano-5-(4-fluoro-phenyl)-2-oxo-cyclohexanecarboxylic acid methyl ester (11) were dissolved in 680 mL of ethanol and 171 mL of concentrated aqueous hydrochloric acid were added. The mixture was heated to reflux for 40 h, then evaporated. The residue was taken up in water and extracted with dichloromethane. The organic layer was washed with brine, dried over magnesium sulphate and evaporated to give 95.2 g of crude product, that was purified by silica gel filtration (heptanes:ethyl acetate) to yield 50.4 g of the desired product 12. Rt=1.26 min (Method 1). Detected mass: 218.2 (M+H+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08541449B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-73d1812c7d0141128be68c792624f4f6 |
| 출처 메모 | uspto-grants-2013_09 |