化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 8-{[(3-Nitroquinolin-4-yl)amino]methyl}-1,4-dioxaspiro[4.5]decan-8-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Chloro-3-nitroquinoline | HCID 11275808 | — |
| 反応物 | 8-(Aminomethyl)-1,4-dioxaspiro[4.5]decan-8-ol | HCID 43436647 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 8-{[(3-Nitroquinolin-4-yl)amino]methyl}-1,4-dioxaspiro[4.5]decan-8-ol | HCID 66919155 | 95.1% |
反応手順
To a 0° C. solution of 4-chloro-3-nitroquinoline (7.50 g, 36.0 mmol) and triethylamine (7.5 mL, 54 mmol) in dichloromethane (150 mL) was added 8-(aminomethyl)-1,4-dioxaspiro[4.5]decan-8-ol (8.10 g, 43.1 mmol). The reaction was allowed to warm to rt and stir overnight, then was concentrated under reduced pressure to yield a yellow solid. The solid was stirred in water (500 mL) and was isolated by filtration, dried under vacuum, and recrystallized from toluene (280 mL) to yield 8-{[(3-nitroquinolin-4-yl)amino]methyl}-1,4-dioxaspiro[4.5]decan-8-ol as bright yellow crystals (12.3 g, 72%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08541438B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-8f8cae2b9bf24dc79721f2f601b073df |
| 出典メモ | uspto-grants-2013_09 |