化工社化工社 化学情報印刷レポート · 研究参考用
2,4,6-Tris(1-methyl-3-trifluoromethylpyrazol-5-yloxy)pyridine → 2,6-Bis(1-methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methoxypyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,4,6-Tris(1-methyl-3-trifluoromethylpyrazol-5-yloxy)pyridine | HCID 15869678 | — |
| 反応物 | Potassium methoxide | HCID 23664618 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2,6-Bis(1-methyl-3-trifluoromethylpyrazol-5-yloxy)-4-methoxypyridine | HCID 22572630 | 43.4% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06130188 |
| 出典データセット | uspto-grants-2000_10 |
| ORD ID | ord-6759362e203b434a933ffc01546fab73 |
| 出典メモ | uspto-grants-2000_10 |