関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 6-Methoxyquinaldine | HCID 70648 | — |
| 反応物 | Diethyl (3-bromopropyl)phosphonate | HCID 283500 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(3-(Diethoxyphosphoryl)propyl)-6-methoxy-2-methylquinolinium bromide | HCID 86639974 | 67.8% |
反応手順
A mixture of 6-methoxy-2-methylquinoline (1.0 g, 5.8 mmol) and diethyl-(3-bromopropyl)-phosphonate (1.6 g, 6.4 mmol) was heated in a pressure tube at 140° C. for 16 hours. The mixture was allowed to cool to room temperature, and the resulting mass was dissolved in DMF (4 mL). The combined mixture was then added dropwise to ethyl acetate (40 mL). Precipitated purple solid was collected by centrifugation, washed with ethyl acetate (3×40 mL) and dried under vacuum to yield 1.7 g of Compound 13 which was then used without any further purification. The structure of Compound 13 is given below:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08476443B2 |
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| 出典データセット | uspto-grants-2013_07 |
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| ORD ID | ord-4b005a1688a141d0ad44724d369ee2cb |
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| 出典メモ | uspto-grants-2013_07 |
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