Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | 4-Chloro-alpha,alpha,alpha-trifluoro-3-nitrotoluene | HCID 8462 | — |
| Edukt | Potassium Hydroxide | HCID 14797 | — |
| Edukt | Benzyldodecyldimethyl ammonium chloride | HCID 53445721 | — |
| Lösungsmittel | 2-Methoxyethanol | HCID 8019 | — |
| Produkt | 2-Nitro-4-(trifluoromethyl)phenol | HCID 9816 | 92% |
Reaktionsschritte
45 g of 4-chloro-3-nitro-benzotrifluoride and 10 ml of 50% strength aqueous benzyldodecyldimethylammonium chloride are initially introduced into 150 ml of ethylene glycol monomethyl ether, and 100 g of 50% strength potassium hydroxide solution are added dropwise in the course of about 30 minutes, up to a temperature of 65° C. The mixture is then stirred at 65° C. for 6 hours and subsequently cooled and rendered acid with concentrated hydrochloric acid, and about 500 ml of distillate are driven over with steam. The organic phase is separated off and washed with 20 ml of dilute hydrochloric acid, and the organic phase is again separated off and dried with sodium sulphate. 38 g of 2-nitro-4-trifluoromethylphenol are obtained, which corresponds to a yield of 92% of theory.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US04225731 |
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| Quelldatensatz | uspto-grants-1980_09 |
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| ORD ID | ord-dd14553770ba48f4a69e66321c63b24e |
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| Quellennotiz | uspto-grants-1980_09 |
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