関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Aminoacetaldehyde dimethyl acetal | HCID 89728 | — |
| 反応物 | Benzene sulphochloride | HCID 22564087 | — |
| 溶媒 | Sodium Carbonate | HCID 10340 | — |
| 生成物 | HCID 3821256 | HCID 3821256 | 101% |
反応手順
56 g 2-aminoacetaldehyde dimethyl acetal are dissolved in 200 ml of a 14 wt. % aqueous sodium carbonate solution at 20° C. in a three-necked flask, equipped with a thermometer, reflux condenser, tap funnel and magnetic stirrer. Subsequently, 88 g benzene sulfochloride are added drop-wise within 1 hour at this temperature under intensive stirring followed by another 2 hours of heating the reaction to 40° to 50° C. mixture under vigorous stirring. After that the intensive smell of benzene sulfochloride has disappeared and a second phase has formed. This heavy oily phase is separated in the separatory funnel, imbibed using diethyl ether and dried over water-free sodium sulfate. Once the drying agent has been removed and the ether has been distilled off, 112 g of the product are obtained (yield: 88% based on the amino acetal used).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05849842 |
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| 出典データセット | uspto-grants-1998_12 |
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| ORD ID | ord-de843fe1380d4fdd9acd7e9e1dac6864 |
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| 出典メモ | uspto-grants-1998_12 |
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