참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | 1,4-Dibromo-2-fluorobenzene | HCID 137004 | — |
| 반응물 | HCID 57440505 | HCID 57440505 | — |
| 생성물 | 1-(4-Acetyl-2-fluorophenyl)ethan-1-one | HCID 22743212 | 100% |
반응 단계
Into a 100 mL single neck flask were placed 1,4-dibromo-2-fluorobenzene (2.35 g, 9.2 mmol), dichlorobis(triphenylphosphine) palladium (II) (0.645 g, 0.92 mmol), tributyt (1-ethoxyvinyl)tin (10 g, 27.7 mmol), in THF (50 mL), and the mixture was heated at reflux while stirring for 18 hours. The reaction was cooled to room temperature and poured into 5N HCl (20 mL). The product was extracted with EtOAc and the organic layer was separated and washed twice with water, dried over anhydrous Na2SO4, filtered, and concentrated under reduced vacuum. The resulting semi-solid was purified via flash chromatography (Silica gel, isocratic) and eluting with a solvent of Hexanes/EtOAc 90:10 to provide the intermediate title compound, 1-(4-acetyl-2-fluorophenyl)ethan-1-one, (1.65 g, 100%) as a solid. Electron spray M.S. 180.9 (M*)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06703425B2 |
|---|
| 출처 데이터셋 | uspto-grants-2004_03 |
|---|
| ORD ID | ord-4641edbb623f42159330a1ff7bd59c50 |
|---|
| 출처 메모 | uspto-grants-2004_03 |
|---|