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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 | HCID 22441681 | HCID 22441681 | — |
| 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 (.060 gram atom) metallic sodium. When the reaction was completed 10.2 g ( b .060 mole) of 3-acetylmercaptocycloheptane 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 (.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 lN HC1 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 | US04062868 |
| 出典データセット | uspto-grants-1977_12 |
| ORD ID | ord-fd65037503514aa684a194251a62a018 |
| 出典メモ | uspto-grants-1977_12 |