関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Dimethylamine, hydrochloride | HCID 10473 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-Ethylpyrrole | HCID 185226 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 1-(1-Ethyl-1H-pyrrol-2-yl)-N,N-dimethylmethanamine | HCID 45088335 | 97% |
反応手順
A mixture of a 35% aqueous formaldehyde solution (9.0 mL, 105 mmol) and dimethylamine hydrochloride (9.0 g, 110 mmol) was added to 1-ethylpyrrol (10.0 g, 105 mmol) under ice-cooling with stirring over 1 hour and 30 minutes and the mixture was stirred at room temperature for 6 hours. A 10% aqueous sodium hydroxide solution (150 mL) and ether were added to the reaction mixture to separate it. The thus obtained organic phase was separated, washed with a saturated aqueous NaCl solution and dried over anhydrous sodium sulfate. After filtration, the solvent was evaporated under reduced pressure and the residue was purified by silica gel chromatography (methylene chloride:methanol, 9:1) to obtain 2-(N,N-dimethylaminomethyl)-1-ethylpyrrol (15.6 9, yield: 97%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07910617B2 |
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| 出典データセット | uspto-grants-2011_03 |
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| ORD ID | ord-eb81db39084e4ab794d972745fa2042f |
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| 出典メモ | uspto-grants-2011_03 |
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