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1-Fluoronaphthalene → 1-(4'-Fluoronaphth-1-yl)-3-methylbutan-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Fluoronaphthalene | HCID 9450 | — |
| 反応物 | Isovaleryl chloride | HCID 66054 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(4'-Fluoronaphth-1-yl)-3-methylbutan-1-one | HCID 59796876 | 87.3% |
反応手順
To an ice/salt cooled solution of 1-fluoronaphthalene (5.1 g) in anhydrous dichloromethane (20 ml) was added aluminium chloride (5.6 g). After 5 minutes, a solution of isovaleryl chloride (4.2 g) in anhydrous dichloromethane (5 ml) was added dropwise over 20 minutes. The mixture was allowed to warm to room temperature overnight, then added cautiously to a vigorously stirred mixture of ice water and dichloromethane. The organic layer was separated, clarified with methanol, washed with brine, dried with sodium sulphate, filtered and evaporated in vacuo. The title compound (7 g) was obtained following silica gel column chromatography of the residue in 20-40% dichloromethane in petroleum ether.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07429607B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-039a8b57ca6e4078848737513c84cff0 |
| 出典メモ | uspto-grants-2008_09 |