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2,4,6-Tris(1-methyl-3-trifluoromethylpyrazol-5-yloxy)pyridine → 2,6-Bis(1-methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methoxypyridine
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 2,4,6-Tris(1-methyl-3-trifluoromethylpyrazol-5-yloxy)pyridine | HCID 15869678 | — |
| 反应物 | 甲醇钾 | HCID 23664618 | — |
| 溶剂 | (5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮 | HCID 887 | — |
| 产物 | 2,6-Bis(1-methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methoxypyridine | HCID 22572630 | 43.4% |
反应步骤
A 3 ml aliquot of a 25 % solution of potassium methylate (10 mmol) in dry methanol is added to a solution of 5.7 g (10 mmol) 2,4,6-tris-(1-methyl-3-trifluoromethylpyrazol-5-yloxy)pyridine in 20 ml anhydrous methanol. After 2 hours at ambient temperature, the reaction mixture is heated to reflux. The solvent is removed under reduced pressure and ethyl acetate is added to the residue. The mixture is washed with a 2 N sodium hydroxide solution. After drying and filtration of the organic layer, the solvents are removed and the residue is washed with diisopropyl ether and pentane. Colorless crystals (1.9 g, 43 % yield) of melting point 107° C. are obtained.
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US06130188 |
| 来源数据集 | uspto-grants-2000_10 |
| ORD ID | ord-6759362e203b434a933ffc01546fab73 |
| 来源说明 | uspto-grants-2000_10 |