関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-Methylpropylenediamine | HCID 13128 | — |
| 反応物 | 4-Chloro-3-nitroquinoline | HCID 11275808 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N1-(3-nitroquinolin-1-yl)-2-methylpropane-1,2-diamine | HCID 86626603 | 99.1% |
反応手順
Under a nitrogen atmosphere, a solution of 1,2-diamino-2-methylpropane (52.20 mL, 503.3 mmol), triethylamine (131.8 mL, 958.8 mmol), and dichloromethane (1.0 L) was chilled in an ice water bath. 4-Chloro-3-nitroquinoline (100.0 g, 479.4 mmol) was added in portions over a period of 5 minutes. The reaction mixture was stirred at 0° C. for 2 hours and then allowed to slowly warm to ambient temperature. After 16 hours the reaction mixture was concentrated under reduced pressure. The residue was triturated with water (500 mL) for 1 hour. The resulting solid was isolated by filtration and dried overnight in a vacuum desiccator to provide 124.6 g of N1-(3-nitroquinolin-1-yl)-2-methylpropane-1,2-diamine as a yellow crystalline solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08846710B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-444e9c8800734027a4b7e3c8451d8e29 |
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| 出典メモ | uspto-grants-2014_09 |
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