関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pentylamine | HCID 8060 | — |
| 反応物 | Triphosgene | HCID 94429 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2-Chloro-4-((6,7-dimethoxyquinazolin-4-yl)oxy)aniline | HCID 21889899 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | N-{2-Chloro-4-[(6,7-dimethoxy-4-quinazolinyl)oxy]phenyl}-N'-pentylurea | HCID 22667094 | 49% |
反応手順
2-Chloro-4-[(6,7-dimethoxy-4-quinazolinyl)oxy]-aniline (50 mg) was dissolved in chloroform (5 ml) and triethylamine (1 ml), and a solution of triphosgene (45 mg) in chloroform was then added to the solution. The mixture was stirred at room temperature for 30 min. Next, amylamine (26 μl) was added to the reaction solution, and the mixture was stirred at room temperature for additional 30 min. A saturated aqueous sodium hydrogencarbonate solution was added to the reaction solution, and the mixture was extracted with chloroform. The chloroform layer was dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure. The residue was purified by HPLC by development with chloroform/methanol to give 33 mg (yield 49%) of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06797823B1 |
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| 出典データセット | uspto-grants-2004_09 |
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| ORD ID | ord-95a4d538c7f6408d9e9ed6b6da4153bb |
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| 出典メモ | uspto-grants-2004_09 |
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