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Sulfuric Acid → (+/-)-cis-1 2-Dimethoxy-4-(2-nitrocyclohex-4-enyl)benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | (+/-)-trans-1,2-DI methoxy-4-(2-nitrocyclohex-4-enyl)benzene | HCID 53874256 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (+/-)-cis-1 2-Dimethoxy-4-(2-nitrocyclohex-4-enyl)benzene | HCID 15389588 | 86% |
反応手順
10.0 g of (+/-)-trans-1,2-dimethoxy-4-(2-nitrocyclohex-4-enyl)benzene and 20.0 g of potassium hydroxide are dissolved in 150 ml of ethanol and 35 ml of dimethylformamide. A solution of 17.5 ml of conc. sulfuric acid in 60 ml of ethanol is then added dropwise such that the internal temperature does not exceed 4° C. After stirring for 1 h, the mixture is added to 1 l of ice-water, the precipitate is filtered off with suction, washed with water and dried and the crude product is recrystallized from ethanol. M.p.: 82.5-84° C.; yield 86% of theory.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06127378 |
| 出典データセット | uspto-grants-2000_10 |
| ORD ID | ord-1c6113ef0cba4125a9bbd14978fd1cc8 |
| 出典メモ | uspto-grants-2000_10 |