関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | Phosphorus pentachloride | HCID 24819 | — |
| 反応物 | 2-Hydroxy-6-methyl-5-nitropyridine | HCID 543053 | — |
| 生成物 | 6-Chloro-2-methyl-3-nitropyridine | HCID 253123 | 182.2% |
反応手順
A mixture of 2-oxo-5-nitro-6-methyl-1,2-dihydropyridine (38.95 g, 253 mmol), phosphorous oxychloride (12.3 mL, 130 mmol), and phosphorous pentachloride (27.9 g, 134 mmol) was heated at 110° C. for 2 hours, whereupon the reaction mixture was charged with an additional portion of phosphorous pentachloride and phosphorous oxychloride (9.9 g and 4.8 mL, respectively). The reaction was stirred 1 hour, then poured into ice-water (600 mL). The brown solid was filtered and washed with cold water, to give 40.88 g of the title compound (94%). MS(m/e): 173 (M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06358972B1 |
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| 出典データセット | uspto-grants-2002_03 |
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| ORD ID | ord-6930c2479e114640abed7a0fbbb21326 |
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| 出典メモ | uspto-grants-2002_03 |
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