関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | HCID 178479710 | HCID 178479710 | — |
| 反応物 | 4-chloro-1-(3-hydroxypropyl)-1H-imidazo[4,5-c]quinolin-2-ol | HCID 178520823 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-chloro-1-(3-chloropropyl)-1H-imidazo[4,5-c]quinolin-2-ol | HCID 178517325 | 64.4% |
反応手順
Phosphorus(III) oxychloride (7.9 g, 52 mmol) was added dropwise to a stirred solution of 4-chloro-1-(3-hydroxypropyl)-1H-imidazo[4,5-c]quinolin-2-ol (12 g, 43 mmol) in DMF (150 mL), and the reaction was stirred overnight at room temperature. An analysis by LC/MS indicated the presence of starting material, and additional phosphorus(III) oxychloride (7.9 g) was added. The reaction was stirred overnight at room temperature and then cooled to approximately 0° C. Water (300 mL) was slowly added, and a precipitate formed. The mixture was stirred for several minutes, and the precipitate was isolated by filtration, washed with water and diethyl ether, and dried in a vacuum oven to provide 8.2 g of 4-chloro-1-(3-chloropropyl)-1H-imidazo[4,5-c]quinolin-2-ol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08088790B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-7e98b61a56564f3c803ac28435001c30 |
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| 出典メモ | uspto-grants-2012_01 |
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