関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 6-Methoxypyridazin-3-amine | HCID 81673 | — |
| 反応物 | 4-((3,5-Dimethylisoxazol-4-yl)methoxy)benzene-1-sulfonyl chloride | HCID 16490702 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | HCID 117925948 | HCID 117925948 | 4.1% |
反応手順
To a solution of 6-methoxypyridazin-3-amine (125 mg, 1.0 mmol) in pyridine (8 mL) at room temperature, was added 4-{[(3,5-dimethyl-4-isoxazolyl)methyl]oxy}benzenesulfonyl chloride (0.302 g, 1.0 mmol). The reaction mixture was stirred at 20° C. for 18 hours. The solvent was evaporated in vacuo and passed through an aminopropyl (NH2) solid phase extraction (SPE) cartridge eluting with methanol, followed by a sulphonic acid (SCX) SPE cartridge eluting with methanol. The crude was then purified by flash silica (Si) chromatography (0-100% ethyl acetate-cyclohexane+0-25% methanol gradient), to provide the title compound (16 mg). LCMS (2 min, formic) Rt 0.83 min, m/z (ES+) 391 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09242972B2 |
|---|
| 出典データセット | uspto-grants-2016_01 |
|---|
| ORD ID | ord-a6f100bcc13f4355b07a0d68d4972464 |
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| 出典メモ | uspto-grants-2016_01 |
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