関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-(4-(Trifluoromethyl)phenyl)ethanamine hydrochloride | HCID 21492969 | — |
| 反応物 | HCID 178457589 | HCID 178457589 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178457593 | HCID 178457593 | — |
反応手順
A stirred mixture of 15.5 g (0.0687 mole) of α-methyl-p-trifluoromethylbenzylamine hydrochloride and 9.55 g (0.0756 mole) of 1-i-propyl-3-cyanoguanidine is immersed in a 190° C oil bath for ten minutes. The melt is cooled to room temperature, dissolved in 100 ml of water, made alkaline with 40% sodium hydroxide solution and extracted twice with 200 ml of ether. The combined ether extracts are dried over potassium carbonate, filtered, and the ether solution made strongly acidic with a saturated ethereal hydrochloric acid ether solution. The precipitate is collected on a filter, washed twice with 50 ml of anhydrous ether, and dried at 40°C/125 mm. for 5 hours. The dihydrochloride is dissolved in 50 ml of water, made strongly alkaline with 40% sodium hydroxide solution, and extracted twice with 100 ml of ether. The combined ether extracts are dried over potassium carbonate, filtered, and the ether solution made strongly acidic with a saturated ethereal hydrochloric acid solution. The precipitate is collected on a filter, washed twice with 50 ml of anhydrous ether, and dried at 40° C/125 mm. to obtain 1-(α-methyl-p-trifluoromethylbenzyl)-5-i-propylbiguanide dihydrochloride.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03996232 |
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| 出典データセット | uspto-grants-1976_12 |
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| ORD ID | ord-318b7b81f1f249558e64ad4b6aac0594 |
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| 出典メモ | uspto-grants-1976_12 |
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