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3-(Trifluoromethyl)phenol → 2-(Methylsulfanyl)-4-[3-(trifluoromethyl)phenoxy]pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-(Trifluoromethyl)phenol | HCID 7376 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Chloro-2-methylthiopyrimidine | HCID 97113 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(Methylsulfanyl)-4-[3-(trifluoromethyl)phenoxy]pyrimidine | HCID 19693871 | — |
反応手順
In THF, a phenoxide was prepared from 3-(trifluoromethyl)phenol (4.54 g, 0.0187×1.5 mol) was mixed with NaH (1.12 g (ca. 60% in mineral oil), 0.0187×1.5 mol), and 4-chloro-2-(methylthio)pyrimidine (Compound No. VII-1) (3.0 g, 0.0187 mol) was added thereto and the mixture was refluxed for about 10 hours. The reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate to separate an organic phase. The organic phase was washed with aqueous saturated sodium chloride, dried over anhydrous sodium sulfate and concentrated, then recrystallized from a methanol/water system to obtain the intermediate compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05723412 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-3d58caaef3e54ab9bff64df1e59b26f5 |
| 出典メモ | uspto-grants-1998_03 |