関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Cyclohexyl bromide | HCID 7960 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | HCID 178524460 | HCID 178524460 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Cyclohexylsulfanyl-nicotinic acid | HCID 28738802 | — |
反応手順
2-Mercapto-nicotinic acid (0.5 g, 3.22 mmol) was dissolved in DMF (5 mL), and the solution was cooled to 0˜5° C. NaH (0.64 g, 16.11 mmol) was added slowly thereto, and the mixture was stirred at 0˜5° C. for 30 minutes. Bromo-cyclohexane (1.19 mL, 9.66 mmol) was added thereto, and the mixture was stirred at room temperature for 12 hours. After the termination of the reaction, the reactant was concentrated under reduced pressure, and the residue was diluted with water. 3N HCl was used to adjust the pH of the solution to 2˜3, and the solution was extracted with EtOAc. The organic layer was dried with MgSO4 and concentrated under reduced pressure to obtain the title compound, which was used in the next step without a separate purification process.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09447044B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-c254a23b3b1a4858b03651e3dddb1ae7 |
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| 出典メモ | uspto-grants-2016_09 |
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