関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Phenol, 4-(aminomethyl)-2-methoxy-, hydrochloride (1:1) | HCID 165576 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Vanillylamine | HCID 70966 | — |
反応手順
The reaction mixture obtained in a) is combined with 38 ml of hydrochloric acid and 6.2 g of Pd/C. Hydrogen is piped into the reaction mixture, with stirring, at 10° C. over a period of 4 hours under a pressure of 4 bar. After the addition of 71 ml of water the mixture is heated to 60° C. and stirred for 1 hour. The catalyst is filtered off and the acetic acid is eliminated from the filtrate by distillation at 60° C. Then the reaction mixture is combined with 141 ml of water in order to dissolve the vanillylamine hydrochloride and the salts and stirred at 60° C. for 0.5 hours. After the addition of 99 ml of hydrochloric acid and stirring for 1 hour, the suspension formed is cooled to 3° C. and after 3 hours the vanillylamine hydrochloride is filtered off, washed with acetone and dried at 50° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06958418B2 |
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| 出典データセット | uspto-grants-2005_10 |
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| ORD ID | ord-7f3ac6f429c74fa8b0b1bdcda7d8dab7 |
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| 出典メモ | uspto-grants-2005_10 |
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