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Ethanol → HCID 178418414、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Methyl 4-oxobut-2-enoate | HCID 111293 | — |
| 反応物 | Pentanimidamide Hydrochloride | HCID 11615174 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | HCID 178418414 | HCID 178418414 | — |
反応手順
Sodium hydride (2.82 g, 0,117 mol) was dissolved in 30 ml of absolute ethanol at 0° C. Valeramidine hydrochloride (16.71 g, 0.123 mol) was added to this solution, and after 15 minutes the solution was filtered and the collected solid was washed with 20 ml of ethanol and 50 ml of benzene. The combined filtrates were diluted with 750 ml of benzene, 15 g (0.117 mol) of methyl 3-formylacrylate was added, and the mixture was refluxed for 18.5 h using a trap to remove water. The solvents were removed under vacuum and the residue slurried in ether. Evaporation of the ether solution gave the title compound as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05728842 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-2843bd13368f422ab3826093b175bc25 |
| 出典メモ | uspto-grants-1998_03 |