化工社化工社 化学情報印刷レポート · 研究参考用
p-Fluoronitrobenzene → methyl-[9-(4-nitrophenyl)-9H-purin-6-yl]amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Fluoronitrobenzene | HCID 9590 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | HCID 178482413 | HCID 178482413 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | methyl-[9-(4-nitrophenyl)-9H-purin-6-yl]amine | HCID 23155308 | 83% |
反応手順
In 120 mL of dimethyl sulfoxide, 10.78 g (80 mmol) of methyl-(9H-purin-6-yl)amine was dissolved, and 1.98 g (82.5 mmol) of sodium hydride (60%) after washing with hexane was added thereto and the mixture solution was stirred at room temperature for one hour. To the reaction solution, 13.0 g (92 mmol) of 4-fluoronitrobenzene was added dropwise and the resulting solution was stirred at 80° C. for two hours. The reaction solution was diluted with 300 mL of water, and the crystal deposited was collected on a filter, then washed with 100 mL of water and subsequently with 500 mL of ethanol, and vacuum dried to obtain 16.14 g (83%) of a target product as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08609656B2 |
| 出典データセット | uspto-grants-2013_12 |
| ORD ID | ord-5751a6afb639405984d55a321dff887b |
| 出典メモ | uspto-grants-2013_12 |