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Sodium hydride → 3-(3,5-Dimethyl-pyrazol-1-yl)-6-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyridazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 3-Chloro-6-(3,5-dimethylpyrazol-1-yl)pyridazine | HCID 321073 | — |
| 反応物 | (5-Methyl-3-phenyl-1,2-oxazol-4-yl)methanol | HCID 2776149 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-(3,5-Dimethyl-pyrazol-1-yl)-6-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-pyridazine | HCID 42629649 | 3.5% |
反応手順
To a solution of (5-methyl-3-phenyl-isoxazol-4-yl)-methanol (76 mg, 0.40 mmol) in DMF (0.8 mL) cooled to 0° C. was added sodium hydride (55% dispersion in mineral oil, 19.2 g, 0.44 mmol). The mixture was stirred at room temperature for 1 h. After addition of 3-chloro-6-(3,5-dimethylpyrazol-1-yl)-pyridazine (91.8 mg, 0.44 mmol) the mixture was stirred at room temperature overnight. Then the mixture was evaporated, extracted (ethyl acetate/water) and the organic phase was dried with sodium sulfate and concentrated. Chromatography (SiO2, heptane:ethanol=100:0 to 95:5) afforded the title compound (5.0 mg, 3%) as a white solid. MS: m/e=362.4 [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-84a12e780d3d4e2a98d86e927a40946f |
| 出典メモ | uspto-grants-2011_05 |