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2-Propanethiol → 2-Isopropylsulfanyl-6-methyl-nicotinic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Propanethiol | HCID 6364 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Methyl 2-chloro-6-methylpyridine-3-carboxylate | HCID 13055804 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Isopropylsulfanyl-6-methyl-nicotinic acid methyl ester | HCID 90118105 | 69.8% |
反応手順
2-Chloro-6-methyl-nicotinic acid methyl ester (1.39 g, 7.44 mmol) obtained in Step A was dissolved in DMF (15 mL). Cs2CO3(4.88 g, 14.99 mmol) and propane-2-thiol (1.39 mL, 14.99 mmol) were added to the solution, and the mixture was stirred at room temperature for 2 hours. The reactant was concentrated under reduced pressure to remove the solvent. The residue was added with water and then extracted with EtOAc. The organic layer was dried with MgSO4, filtered and concentrated under reduced pressure. The obtained residue was purified by column chromatography (eluent EtOAc/Hex=1/5) to obtain the title compound (1.17 g, 69%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09447044B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-7ad44a8f9f314848acf3a650ee093685 |
| 出典メモ | uspto-grants-2016_09 |