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Benzylamine → (7-Methoxy-3,4-dihydronaphthalen-1-yl)acetonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzylamine | HCID 7504 | — |
| 反応物 | Heptanoic Acid | HCID 8094 | — |
| 反応物 | Cyanoacetic acid | HCID 9740 | — |
| 反応物 | 7-Methoxy-1,2,3,4-tetrahydronaphthalen-1-one | HCID 81276 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | (7-Methoxy-3,4-dihydronaphthalen-1-yl)acetonitrile | HCID 11287102 | 90% |
反応手順
There are introduced into a 670 litre reactor 85.0 kg of 7-methoxy-1-tetralone, 60.3 kg of cyanoacetic acid and 15.6 kg of heptanoic acid in toluene in the presence of 12.7 kg of benzylamine. The mixture is heated at reflux. When all the starting substrate has disappeared, the solution is cooled and filtered. The precipitate obtained is washed with toluene and then the filtrate obtained is washed with a 2N sodium hydroxide solution and subsequently with water until neutral. After removal of the solvent by evaporation, the resulting solid is recrystallised from an ethanol/water (80/20) mixture to give the title product in a yield of 90% and with a chemical purity exceeding 99%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07250531B2 |
| 出典データセット | uspto-grants-2007_07 |
| ORD ID | ord-24f97e0aa3524bb0b34c5d7adcebb673 |
| 出典メモ | uspto-grants-2007_07 |