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 | 1-Ethylpyrrole | HCID 185226 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | 1-(1-Ethyl-1H-pyrrol-2-yl)-N,N-dimethylmethanamine | HCID 45088335 | 97.6% |
反応手順
A mixture of 35% aqueous formaldehyde solution (9 ml, 105 mmol) and dimethylamine hydrochloride (9.0 g, 110 mmol) was added to 1-ethylpyrrole (10.0 g, 105 mmol) with stirring under ice-cooling over a 90-minute interval, and then the resulting mixture was stirred at room temperature for 6 hours. After stirring, 10% aqueous sodium hydroxide solution (150 ml) was added to the reaction mixture, and the resulting mixture was extracted with ether. The extract was washed with saturated aqueous sodium chloride solution and dried over anhydrous sodium sulfate. After filtration, the solvent was removed in vacuo, and the residue was purified by chromatography on a silica gel column using a mixed solvent of dichloromethane and methanol (9:1) as the eluent to afford 2-(N,N-dimethylaminomethyl)-1-ethylpyrrole (15.6 g, yield: 97%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08101650B2 |
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| 出典データセット | uspto-grants-2012_01 |
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| ORD ID | ord-0aedc09244284387a47658bd2aa45e94 |
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| 出典メモ | uspto-grants-2012_01 |
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