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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 (compound I1) 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 in ethanol. 8.6 g of the title compound of m.p. 82.5-84° C. are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08202880B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-430d3098996d4ef78351fa10f3406af0 |
| 出典メモ | uspto-grants-2012_06 |