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Sodium hydride → 6-(5-Methyl-3-phenyl-isoxazol-4-ylmethoxy)-[1,2,4]triazolo[4,3-b]pyridazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 6-Chloro-[1,2,4]triazolo[4,3-b]pyridazine | HCID 313624 | — |
| 反応物 | (5-Methyl-3-phenyl-1,2-oxazol-4-yl)methanol | HCID 2776149 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-(5-Methyl-3-phenyl-isoxazol-4-ylmethoxy)-[1,2,4]triazolo[4,3-b]pyridazine | HCID 42630249 | 51% |
反応手順
To a solution of (5-methyl-3-phenyl-isoxazol-4-yl)-methanol (100 mg, 0.53 mmol) in DMF (2 mL) was added sodium hydride (55% dispersion in mineral oil, 25.4 mg, 0.58 mmol). The mixture was stirred at room temperature for 15 min. After addition of 6-chloro-1,2,4-triazolo[4,3-b]pyridazine (90 mg, 0.58 mmol) the mixture was stirred at room temperature for another 2 h. Then the mixture was evaporated, extracted (ethyl acetate/water) and the organic phase was dried with sodium sulfate and concentrated. Chromatography (SiO2, dichloromethane:methanol=100:0 to 9:1) afforded the title compound (80 mg, 51%) as a white solid. MS: m/e=308.4 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07943619B2 |
| 出典データセット | uspto-grants-2011_05 |
| ORD ID | ord-92ae9d6cfb8e4f08b0f53649947e0ec7 |
| 出典メモ | uspto-grants-2011_05 |