関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Propylamine | HCID 7852 | — |
| 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 | Krn-633 | HCID 9549295 | 64.2% |
反応手順
2-Chloro-4-[(6,7-dimethoxy-4-quinazolinyl)oxy]-aniline (5.13 g) was dissolved in chloroform (100 ml) and triethylamine (50 ml), and a solution of triphosgene (4.59 g) in chloroform (3 ml) was then added to the solution. The mixture was stirred for 30 min. Next, n-propylamine (2.74 g) was added to the reaction solution, and the mixture was stirred for additional 2 hr. 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 chromatography on silica gel by development with chloroform/methanol (50/1) to give 4.14 g (yield 64%) 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-0073c2ec341e43cd829951c7f144b812 |
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| 出典メモ | uspto-grants-2004_09 |
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