関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | p-Bromobenzenesulfonyl chloride | HCID 7396 | — |
| 反応物 | 1-Methylpiperazine | HCID 53167 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(4-Bromophenylsulfonyl)-4-methylpiperazine | HCID 710729 | — |
反応手順
A solution of 4-bromobenzene-1-sulfonyl chloride (256 mg, 1.00 mmol) in 1 mL of dichloromethane was slowly added to a vial (40 mL) containing 5 mL of a saturated aqueous solution of sodium bicarbonate, dichloromethane (5 mL) and 1-methylpiperazine (100 mg, 1.00 mmol). The reaction was stirred at room temperature overnight. The phases were separated and the organic layer was dried over magnesium sulfate. Evaporation of the solvent under reduced pressure provided the required product, which was used in the next step without further purification. ESI-MS m/z calc. 318.0. found 318.9 (M+1)+. Retention time of 1.30 minutes. 1H NMR (300 MHz, CDCl3) δ 7.65 (d, J=8.7 Hz, 2H), 7.58 (d, J=8.7 Hz, 2H), 3.03 (t, J=4.2 Hz, 4H), 2.48 (t, J=4.2 Hz, 4H), 2.26 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07741321B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-98148ec2c0304d52aa28b7f15b9bb935 |
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| 出典メモ | uspto-grants-2010_06 |
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