関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,4,5-Trichlorophenol | HCID 7271 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Ethyl 5-chloro-2-nitrobenzoate | HCID 603450 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | Ethyl 5(2,4,5-trichlorophenoxy)-2-nitrobenzoate | HCID 21287084 | 38.8% |
反応手順
2,4,5-Trichlorophenol (20 g) in dry dimethylacetamide (40 ml) was treated with sodium hydride (5.28 g of 50% dispersion in oil) in portions and the resulting mixture heated to 120° C. Ethyl-5-chloro-2-nitrobenzoate (16.5 g) was added in solution in dry dimethylacetamide (60 ml) and the mixture heated at 160° C. for ten hours. The solvent was removed and the residue washed with water and extracted with ether. The ether solution was extracted with ether. The ether solution was evaporated. The remaining oil solidified and was recrystallised from ethanol to give ethyl 5(2,4,5-trichlorophenoxy)-2-nitrobenzoate (10.9 g) with a melting point of 99°-102° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04465508 |
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| 出典データセット | uspto-grants-1984_08 |
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| ORD ID | ord-61b2158dbd114476afce0389eb0a81b9 |
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| 出典メモ | uspto-grants-1984_08 |
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