関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Hydroxypyridine | HCID 7971 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 5-(2-Chloro-4-(trifluoromethyl)phenoxy)-2-nitrobenzoyl chloride | HCID 3017765 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3-Pyridyl 5-[2-chloro-4-(trifluoromethyl)phenoxy]-2-nitrobenzoate | HCID 13475656 | 70.7% |
反応手順
To a stirred solution of 5-[2-chloro-4-(trifluoromethyl)phenoxy]-2-nitrobenzoyl chloride (3.79 g, 0.01 mole) and triethyl amine (1.01 g, 0.01 mole) in toluene (50 ml) was added 3-hydroxypyridine (0.95 g, 0.01 mole). The temperature exothermed to 33° C. and there was an immediate precipitate. The reaction was then refluxed for 24 hours, cooled to room temperature and the triethylamine hydrochloride precipitate collected by filtration. The toluene solution was washed with dilute sodium hydroxide solution and then with saturated sodium chloride solution. After drying and evaporation of the solvent there was obtained 3.1 g of brown oil which solidified. This was triturated with hexane and the solid filtered and dried to give a tan product, m.p. 65°-68° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04517010 |
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| 出典データセット | uspto-grants-1985_05 |
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| ORD ID | ord-db7961b217924eacadb71753c875ceb0 |
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| 出典メモ | uspto-grants-1985_05 |
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