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Pyridine → 5-Chloro-thiophene-2-sulfonic acid (3-methyl-bicyclo[3.2.1]oct-8-yl)-amide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 5-Chlorothiophene-2-sulfonyl chloride | HCID 2733925 | — |
| 反応物 | 3-Methyl-bicyclo[3.2.1]oct-8-ylamine | HCID 17986049 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-Chloro-thiophene-2-sulfonic acid (3-methyl-bicyclo[3.2.1]oct-8-yl)-amide | HCID 59701883 | 10% |
反応手順
3-Methyl-bicyclo[3.2.1]oct-8-ylamine (prepared in Step 2, 0.165 mmol) was dissolved in DCM (1.5 mL) and treated with 5-chlorothiophenesulphonyl chloride (53.7 mg, 0.248 mmol) followed by pyridine (100 μL). The reaction was stirred at room temperature for 66 h, followed by heating at 60° C. for 18 h. The reaction mixture was evaporated and purified by mass-directed preparative HPLC to give the desired product (5.3 mg, 10%) as a mixture of four isomers. m/z 320 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07365196B2 |
| 出典データセット | uspto-grants-2008_04 |
| ORD ID | ord-f426eb8f5f864e4fa84cba3b80e03055 |
| 出典メモ | uspto-grants-2008_04 |