関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Fluorobenzene | HCID 10008 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 3-Pyridinecarbonyl chloride, hydrochloride (1:1) | HCID 88438 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 生成物 | (4-Fluorophenyl)(pyridin-3-yl)methanone | HCID 762660 | — |
反応手順
To a suspension of 140 g of nicotinic acid chloride hydrochloride in 500 ml of fluorobenzene cooled to 0° C. are added 280 g of aluminium chloride portionwise. The mixture is held under reflux for 6 hours, cooled and then poured onto ice. After the addition of sodium hydroxide up to pH=8, the mixture is extracted with dichloromethane. The organic phase is dried over magnesium sulphate and then evaporated under vacuum. The residue crystallises in a pentane/diisopropyl ether mixture giving 108.5 g of 3-(4-fluorobenzoyl)pyridine in the form of crystals melting at 91° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06180651B2 |
|---|
| 出典データセット | uspto-grants-2001_01 |
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| ORD ID | ord-ffe533d9ce28413ca8cbdc337e853fb3 |
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| 出典メモ | uspto-grants-2001_01 |
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