関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Potassium Chlorate | HCID 6426889 | — |
| 反応物 | HCID 178526703 | HCID 178526703 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178526838 | HCID 178526838 | — |
反応手順
Concentrated hydrochloric acid (239 g) was added to 2-hydroxy-5-nitropyridine (40.0 g). The resulting slurry was heated to 53° C., and stirred until all the solids dissolved. To this was slowly added a solution of potassium chlorate (14.0 g) in water (250 g), while maintaining the temperature between 55° C. and 59° C. The resulting mixture was stirred at 58-62° C. for about 1 hour. The reaction was then cooled to room temperature, stirred for 12 hours and then filtered. After washing the wet cake with water, the product was dried in a vacuum oven. 1H NMR (400 MHz/DMSO-d6) δ 8.64 (d, J=2.9 Hz, 1H), 8.35 (d, J=2.9 Hz, 1H)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07902371B2 |
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| 出典データセット | uspto-grants-2011_03 |
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| ORD ID | ord-492c546b2d804bae9106948c18fa0755 |
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| 出典メモ | uspto-grants-2011_03 |
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