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2,2,2-Trifluoroethanol → 2-Methylthio-4-(2,2,2-trifluoroethoxy)pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,2,2-Trifluoroethanol | HCID 6409 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Chloro-2-methylthiopyrimidine | HCID 97113 | — |
| 反応物 | Ammonia chloride | HCID 20976574 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Methylthio-4-(2,2,2-trifluoroethoxy)pyrimidine | HCID 19694186 | 73.1% |
反応手順
2,2,2-Trifluoroethanol (3.74 g) was dissolved in N,N-dimethylformamide (50 mL), sodium hydride (about 60% in oil) (1.37 g) was added under ice-cooling, and the mixture was stirred at room temperature for 20 min. After ice-cooling again, 4-chloro-2-(methylthio)pyrimidine (5.0 g) was added, and the mixture was stirred at 0° C. for 1 hr. Saturated aqueous ammonia chloride solution was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure to give the title compound (5.1 g) as a slightly yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08026370B2 |
| 出典データセット | uspto-grants-2011_09 |
| ORD ID | ord-9ce47e7d2d1247d6902f1a737bec97b1 |
| 出典メモ | uspto-grants-2011_09 |