関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Cyanobenzene-1-sulfonyl chloride | HCID 2801360 | — |
| 反応物 | Dimethylamine methanol | HCID 22497844 | — |
| 生成物 | 3-(Aminomethyl)-N,N-dimethylbenzenesulfonamide | HCID 16795356 | — |
反応手順
(Step 1) To a 2M dimethylamine methanol solution (3.7 ml) was added 3-cyanobenzenesulfonyl chloride (1.5 g) at 0° C., and the mixture was stirred at room temperature for 2 hr. The solvent was evaporated under reduced pressure, saturated brine was added, and the mixture was extracted with ethyl acetate. The solvent was evaporated under reduced pressure. 10% Palladium carbon powder (0.79 g) was added to a solution (10 ml) of the residue in ethanol, and the mixture was stirred overnight under a hydrogen atmosphere (1 atm). The solution was filtered through celite. The solvent was evaporated under reduced pressure. The residue was purified by basic silica gel column chromatography (ethyl acetate) to give 3-(aminomethyl)-N,N-dimethylbenzenesulfonamide (1.0 g) as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07982044B2 |
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| 出典データセット | uspto-grants-2011_07 |
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| ORD ID | ord-d4a654760e464f70966b607d110a5721 |
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| 出典メモ | uspto-grants-2011_07 |
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