関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Benzenesulfonyl chloride | HCID 7369 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1,3-Cyclohexanediamine | HCID 18814 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (3-Aminocyclohexyl)(phenylsulfonyl)amine | HCID 22714123 | — |
反応手順
A solution of 1,3-diaminocyclohexane (1.14 g, 10 mmol, undetermined isomer mixture) in methylene chloride (50 mL) was cooled to 0° C. and phenylsulfonyl chloride (0.64 mL, 5 mmol) was added dropwise. The mixture was stirred at 0° C. for 4 h, then 1N sodium hydroxide solution (10 mL) was added and the mixture stirred an additional 5 min. The phases were separated, the organic phase was dried (K2CO3), filtered, and concentrated in vacuo. Toluene was added and the mixture re-concentrated to remove any remaining diamine, to give 0.77 g of a semi solid. 1H—NMR was consistent with the desired structure. MS (ion spray) 255 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06743794B2 |
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| 出典データセット | uspto-grants-2004_06 |
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| ORD ID | ord-00c7fddcef0447a38fcc09444aa75ea4 |
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| 出典メモ | uspto-grants-2004_06 |
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