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2-(Methylthio)benzimidazole → 1-(4,6-Dimethoxypyrimidin-2-yl)-2-methylthiobenzimidazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-(Methylthio)benzimidazole | HCID 23539 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4,6-Dimethoxy-2-(methylsulfonyl)pyrimidine | HCID 838363 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(4,6-Dimethoxypyrimidin-2-yl)-2-methylthiobenzimidazole | HCID 12056928 | 86.9% |
反応手順
2-Methylthiobenzimidazole (0.50 g) was dissolved in dimethylformamide (10 ml), and sodium hydride (60% purity, oily) (0.13 g) was added thereto at room temperature. After stirring for 1 hour, 2-methylsulfonyl-4,6-dimethoxypyrimidine (0.67 g) was added at room temperature, followed by stirring for 8 hours. Ice water was added, followed by extraction with ethyl acetate, washing with a saturated sodium chloride aqueous solution and drying over anhydrous magnesium sulfate. The solvent was distilled off, and the residue was purified by silica gel column chromatography to obtain 0.80 g of the desired product as a white powder (m.p. 135-137° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06872729B2 |
| 出典データセット | uspto-grants-2005_03 |
| ORD ID | ord-37bb7a63f4864f6d82b49b13368259a3 |
| 出典メモ | uspto-grants-2005_03 |