関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 2-Bromo-5-nitrothiazole | HCID 18211 | — |
| 反応物 | Chloropyrazine | HCID 73277 | — |
| 反応物 | Sodium sulfide nonahydrate | HCID 73972 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | ((5-nitro-2-thiazolyl)thio)Pyrazine | HCID 20386480 | 72% |
反応手順
To a solution of 60.0 g (0.25 mol) of sodium sulfide nonahydrate in 500 ml of dimethyl formamide was gradually added 29 g (0.25 mol) of chloropyrazine in 100 ml of dimethyl formamide. The solution was stirred overnight at approximately 40° C. following which 52.5 g (0.25 mol) of 2-bromo-5-nitrothiazole was added as a solid. This reaction mixture was stirred at room temperature for 4 hours. After this period it was poured into water. The resulting precipitate was collected by suction filtration, washed with water and dried. The crude product was crystallized from methanol to yield 38 g (72% yield) of yellowish-gold crystals, m.p. 129°-130° C. A sample was subjected to elemental analysis. The results obtained were as follows:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04174394 |
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| 出典データセット | uspto-grants-1979_11 |
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| ORD ID | ord-d6a3df8b95524e459345095859e7e471 |
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| 出典メモ | uspto-grants-1979_11 |
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