関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1,3-Dioxolane-4-methanamine, 2,2-dimethyl- | HCID 4122349 | — |
| 反応物 | 7-(Benzyloxy)-4-chloro-3-nitroquinoline | HCID 21075751 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (7-Benzyloxy-3-nitro-quinolin-4-yl)[(2,2-dimethyl[1,3]dioxolan-4-yl)methyl]amine | HCID 67051130 | 96.2% |
反応手順
Triethylamine (31.88 mL, 228.77 mmol) followed by 2,2-dimethyl-1,3-dioxolan-4-methanamine (20.0 g, 152.51 mmol) were added to a solution of 7-benzyloxy-4-chloro-3-nitroquinoline (48.00 g, 152.51 mmol) in dichloromethane (400 mL), which was then stirred at ambient temperature for 6 hours. The crude reaction mixture was concentrated under reduced pressure, and the resulting solid was treated with water. The mixture was stirred for 1 hour. The solid was collected by filtration, washed with water, dried, suspended in diethyl ether (400 mL), sonicated, and the resulting precipitate material was collected by filtration. The product was dried under vacuum at 40° C. for 12 hours to afford 60.1 g of (7-benzyloxy-3-nitro-quinolin-4-yl)[(2,2-dimethyl[1,3]dioxolan-4-yl)methyl]amine as a yellow solid, mp 154-155° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09365567B2 |
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| 出典データセット | uspto-grants-2016_06 |
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| ORD ID | ord-5883e65dd3034f049a762908c792b7cf |
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| 出典メモ | uspto-grants-2016_06 |
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