関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tert-Butylamine | HCID 6385 | — |
| 反応物 | 3-Chloropropanesulphonyl chloride | HCID 15410 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-tert-butyl-3-chloropropane-1-sulfonamide | HCID 11701296 | 99% |
反応手順
tert-Butylamine (3.0 mol, 315.3 mL) was dissolved in THF (2.5 L). The solution was cooled to −20° C. 3-Chloropropanesulfonyl chloride (1.5 mol, 182.4 mL) was added slowly. The reaction mixture was allowed to warm to rt and stirred for 24 h. The mixture was filtered, and the filtrate was concentrated in vacuo. The residue was dissolved in CH2Cl2 (2.0 L). The resulting solution was washed with 1 N HCl (1.0 L), water (1.0 L), brine (1.0 L) and dried over Na2SO4. It was filtered and concentrated in vacuo to give a slightly yellow solid, which was crystallized from hexane to afford the product as a white solid (316.0 g, 99%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07741281B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-4d152abc044543a395564c614ea0d57a |
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| 出典メモ | uspto-grants-2010_06 |
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