関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Chloropropanesulphonyl chloride | HCID 15410 | — |
| 反応物 | 2,4-Dimethoxybenzylamine hydrochloride | HCID 3084343 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 63362723 | HCID 63362723 | — |
反応手順
To a solution of 2,4-dimethoxy-benzylamine hydrochloride (1 eq.) and TEA (2 eq.) in DCM was added dropwise at 0° C. a solution of 3-chloro-propane-1-sulfonyl chloride (1 eq.) in DCM. The reaction was stirred at 20° C. for 20 h. The crude was diluted with DCM, washed twice with water, twice with aqueous HCl (0.1N) and twice with a saturated aqueous solution of NaHCO3. The organic layer was dried over MgSO4, filtered and concentrated under reduced pressure. The crude was purified by chromatography on silica gel (elution with heptane/EtOAc: 100/0 to 20/80) to afford 3-chloro-propane-1-sulfonic acid 2,4-dimethoxy-benzylamide.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08759334B2 |
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| 出典データセット | uspto-grants-2014_06 |
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| ORD ID | ord-e4ec7a6c826a4b9f8a59e6093972de0c |
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| 出典メモ | uspto-grants-2014_06 |
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