HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sulfuric Acid → (+/-)-cis-1 2-Dimethoxy-4-(2-nitrocyclohex-4-enyl)benzene
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sulfuric Acid | HCID 1118 | — |
| Edukt | Potassium Hydroxide | HCID 14797 | — |
| Edukt | (+/-)-trans-1,2-DI methoxy-4-(2-nitrocyclohex-4-enyl)benzene | HCID 53874256 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | (+/-)-cis-1 2-Dimethoxy-4-(2-nitrocyclohex-4-enyl)benzene | HCID 15389588 | 86% |
Reaktionsschritte
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.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08202880B2 |
| Quelldatensatz | uspto-grants-2012_06 |
| ORD ID | ord-430d3098996d4ef78351fa10f3406af0 |
| Quellennotiz | uspto-grants-2012_06 |