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Water → 2-Chloro-3-(4-phenylbenzoyl)-pyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Biphenyl | HCID 7095 | — |
| 反応物 | 2-Chloronicotinoyl chloride | HCID 2774541 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Carbon Disulfide | HCID 6348 | — |
| 生成物 | 2-Chloro-3-(4-phenylbenzoyl)-pyridine | HCID 20145720 | — |
反応手順
26.7 g AlCl3 is added slowly while stirring to a solution of 9.2 g biphenyl and 10.6 g 2-chloronicotinoyl chloride in 170 ml carbon disulfide. The mixture is refluxed 5 hrs. After cooling, the S2C layer is poured off, and the residue is added to acidic ice: water, basified and extracted with methylene chloride. The combined extracts are washed, dried (MgSO4) and solvent removed in vacuo. The crude product is chromatographed on a silicagel column and eluted with benzene:ethyl acetate 15:1. Yield: 5 g of title product, m.p. 128°-32° C.; UV (ethanol): λmax. 295 nm, ε: 27,260; Cl 11.96 (12.07).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04614833 |
| 出典データセット | uspto-grants-1986_09 |
| ORD ID | ord-690af17d6aae405db2f26be15c8d485b |
| 出典メモ | uspto-grants-1986_09 |