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3-(Trifluoromethyl)phenol → 2-(Methylsulfanyl)-4-(trifluoromethyl)-6-[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-(methylsulfanyl)-6-(trifluoromethyl)pyrimidine | HCID 248063 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-(Methylsulfanyl)-4-(trifluoromethyl)-6-[3-(trifluoromethyl)phenoxy]pyrimidine | HCID 1475000 | — |
反応手順
m-(Trifluoromethyl)phenol (1.06 g, 0.0044×1.5 mol) and NaH (0.26 g (ca.60% in mineral oil), 0.0044×1.5 mol) were dissolved in THF, and then 4-chloro-2-methylthio-6-(trifluoromethyl)pyrimidine (Compound No. VII-17) (1.0 g, 0.0044 mol) was added thereto. The resulting solution was refluxed for about 7 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. Thereafter, remaining phenol and others were distilled off in a tubular oven (under water flow, 150° C.) 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-779700042b074f55b42f3a2202e7c555 |
| 出典メモ | uspto-grants-1998_03 |