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Ethylamine hydrochloride → 3-chloro-N-methylpropane-1-sulfonamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethylamine hydrochloride | HCID 11198 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Chloropropanesulphonyl chloride | HCID 15410 | — |
| 触媒 | Benzyltrimethylammonium chloride | HCID 5963 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-chloro-N-methylpropane-1-sulfonamide | HCID 10241253 | 74% |
反応手順
3-Chloropropylsulfonyl chloride 1 (16.8 g, 94.9 mmol), ethylamine hydrochloride (13.5 g, 200 mmol), and potassium carbonate (27.6 g, 200 mmol) were sequentially added to ethyl acetate (500 ml). After the addition of N-benzyltrimethylammonium chloride (about 200 mg) to the mixture, the resultant mixture was stirred for 2 hours at room temperature and dried over anhydrous sodium sulfate. The mixture was filtered through a small amount of silica gel and the filtrate was concentrated in vacuo to give 12 g (74%) of crude N-methyl-3-chloropropylsulfonamide (intermediate 3b) as a pale yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06743923B2 |
| 出典データセット | uspto-grants-2004_06 |
| ORD ID | ord-90f0a7066fb64014b0743cd036393fb5 |
| 出典メモ | uspto-grants-2004_06 |