関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Biphenyl | HCID 7095 | — |
| 反応物 | 4-Fluorobenzoyl chloride | HCID 67879 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | 1,2,3-Trichlorobenzene | HCID 6895 | — |
| 生成物 | ([1,1'-Biphenyl]-4-yl)(4-fluorophenyl)methanone | HCID 14549661 | 47% |
反応手順
To a stirred solution of biphenyl (96.02 g, 0.632 mol) in trichlorobenzene (640 mL) was added aluminium chloride (91 g, 0.174 mol) in two portions. 4-Fluorobenzoyl chloride (70 mL, 0.593 mol) was then added dropwise from a dropping funnel over 1 h to the solution at 40° C., and the temperature was then raised to 100° C. for 6 h until HCl ceased to evolve. The mixture was allowed to cool to room temperature and poured into an ice/HCl mixture (ca. 2 L), and left stirring overnight. The water was decanted and the white sludge was stirred vigorously with methanol. The crude product was recovered by filtration, washed with methanol, and then dried under vacuum at 80° C. overnight This product (110 g) was recrystallised twice from toluene to give white crystals of 4-(4′-fluorobenzoyl)biphenyl (77 g, 47%); m.p. 149° C. (lit. 148.5-149° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07736539B2 |
|---|
| 出典データセット | uspto-grants-2010_06 |
|---|
| ORD ID | ord-5f9cd88336b0483b803cb3d6ee742276 |
|---|
| 出典メモ | uspto-grants-2010_06 |
|---|