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2-Naphthalenecarboxaldehyde → Ethyl 2-methyl-3-beta-naphthyl-acrylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Naphthalenecarboxaldehyde | HCID 6201 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Butanedioic acid, 2-methyl-3-oxo-, 1,4-diethyl ester | HCID 97750 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | Ethyl 2-methyl-3-beta-naphthyl-acrylate | HCID 54219653 | 45.2% |
反応手順
40 g (0.2 mol) of ethyl α-ethoxalylpropionate are added to a suspension of 5.5 g (0.2 mol) of 80% strength sodium hydride in 300 ml of absolute xylene at 70° C. When the evolution of hydrogen has ended, 31.2 g (0.2 mol) of β-naphthaldehyde, dissolved in xylene, are added dropwise, and when the addition has ended the mixture is heated at the boiling point for 90 minutes. 150 ml of water are added to the cooled reaction mixture and the organic phase is separated off, washed with 7% strength sodium carbonate solution, dried over sodium sulphate and concentrated. The residue is distilled in vacuo. 21.7 g (45.2% of theory) of ethyl 2-methyl-3-β-naphthyl-acrylate of boiling point 110° C./0.13 mbar are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04829063 |
| 出典データセット | uspto-grants-1989_05 |
| ORD ID | ord-0c9096043ec04b518637325bc83c8365 |
| 出典メモ | uspto-grants-1989_05 |