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Sodium → 3-[(2-Nitroethyl)sulfanyl]cyclohept-1-ene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | 2-nitroethyl Acetate | HCID 11815399 | — |
| 反応物 | 3-Acetylmercaptocycloheptene | HCID 12620959 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3-[(2-Nitroethyl)sulfanyl]cyclohept-1-ene | HCID 12621009 | 99.4% |
反応手順
To 40 ml of absolute ethanol was added 1.38 g (0.060 gram atom) metallic sodium. When the reaction was completed, 10.2 g (0.060 mole) of 3-acetylmercaptocycloheptene in 20 ml of absolute ethanol was added and the reaction mixture was brought up to reflux for 15 minutes. The solution was then cooled to 0° and 7.98 g (0.060 mole) of 1-nitro-2-acetoxyethane in 20 ml absolute ethanol was added. The reaction was allowed to proceed for 3.0 hours at 0° and then was partitioned between 1 N HCl and methylene chloride. The aqueous phase was further extracted with methylene chloride. The organic phases were pooled, dried over sodium sulfate, and evaporated to afford 12 g (99%) of pure 3-[2-nitroethylthio]cycloheptene as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04175086 |
| 出典データセット | uspto-grants-1979_11 |
| ORD ID | ord-a8fed77ef40e48b4850d99848d9e4d07 |
| 出典メモ | uspto-grants-1979_11 |