化工社化工社 化学情報印刷レポート · 研究参考用
Di-(2-nitroisobutyl)amine → Bis(2-amino-2-methylpropyl)amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Di-(2-nitroisobutyl)amine | HCID 21951119 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Bis(2-amino-2-methylpropyl)amine | HCID 226845 | 52% |
反応手順
Into a 2 L pressure reactor, 21.17 g (0.0965 mol) of compound III was placed along with 600 mL of ethanol (90%). Approximately 3 g of Raney Nickel was added and the bomb was pressurized to 90 PSI with hydrogen (99.9%). The solution was stirred and intermittently repressurized with hydrogen. Over the course of 5 days, 105 PSI (0.406 mol) of hydrogen were consumed. The bomb was then depressurized and the solution filtered through celite to remove the catalyst. The filtrate was evaporated under vacuum to remove all solvent and then was vacuum distilled at room temperature and a pressure of 50 mtorr. Purified product weighed 8.031 g, giving a yield of 52%. Purity was checked by NMR, with a singlet at 2.26 ppm and a singlet at 0.96 ppm.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09029189B2 |
| 出典データセット | uspto-grants-2015_05 |
| ORD ID | ord-5fd45ad2e1874859bcba9fbdb89c970a |
| 出典メモ | uspto-grants-2015_05 |