関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 4-(2-(Diethylamino)-Ethoxy)-Benzaldehyde | HCID 411674 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | {4-[2-(Diethylamino)ethoxy]phenyl}methanamine | HCID 235944 | 65% |
反応手順
To the solution of 4-diethylaminoethoxybenzaldehyde X in 180 ml 10% solution of ammonia in anhydrous ethanol, 4.5 g RaNi was added and the mixture was heated to 80° C. at the pressure 68 atm in the autoclave under hydrogen input to the reaction mixture under stirring for 12 hours. The mixture was cooled, the catalyst was filtered off, washed with ethanol. The solvent was distilled off from the solution and the distillation residue was purified by distillation under the reduced pressure. Afforded 13 g (65%) of 4-diethylaminoethoxybenzylamine XI. Colourless fluid 138-140° C./0.5 torr, n20D=1.520. Lit. [6.7] reports 130° C./0.3 torr, n20D=1.5220.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08193184B2 |
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| 出典データセット | uspto-grants-2012_06 |
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| ORD ID | ord-854c51b8d09f40c48d3a03ca81d923d3 |
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| 出典メモ | uspto-grants-2012_06 |
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