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间三氟甲基苯酚 → 2-(Methylsulfanyl)-4-(trifluoromethyl)-6-[3-(trifluoromethyl)phenoxy]pyrimidine
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 间三氟甲基苯酚 | HCID 7376 | — |
| 反应物 | 氢化钠 | HCID 24758 | — |
| 反应物 | 4-氯-2-甲硫基-6-三氟甲基嘧啶 | HCID 248063 | — |
| 溶剂 | 四氢呋喃 | HCID 8028 | — |
| 产物 | 2-(Methylsulfanyl)-4-(trifluoromethyl)-6-[3-(trifluoromethyl)phenoxy]pyrimidine | HCID 1475000 | — |
反应步骤
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.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US05723412 |
| 来源数据集 | uspto-grants-1998_03 |
| ORD ID | ord-779700042b074f55b42f3a2202e7c555 |
| 来源说明 | uspto-grants-1998_03 |