関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Chloro-alpha,alpha,alpha-trifluoro-3-nitrotoluene | HCID 8462 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Benzyldodecyldimethyl ammonium chloride | HCID 53445721 | — |
| 溶媒 | 2-Methoxyethanol | HCID 8019 | — |
| 生成物 | 2-Nitro-4-(trifluoromethyl)phenol | HCID 9816 | 92% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04225731 |
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| 出典データセット | uspto-grants-1980_09 |
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| ORD ID | ord-dd14553770ba48f4a69e66321c63b24e |
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| 出典メモ | uspto-grants-1980_09 |
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