関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-Bromo-5-hydroxypyridine | HCID 599529 | — |
| 反応物 | 1-(4-Fluorobenzenesulfonyl)pyrrolidine | HCID 796578 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | 3-Bromo-5-(4-(pyrrolidine-1-sulfonyl)phenoxy)pyridine | HCID 21964095 | 59.1% |
反応手順
A mixture of 5-bromo-3-pyridinol (2.61 g, 15 mmol), dimethylacetamide (50 mL), 1-((4-fluorophenyl)sulfonyl)pyrrolidine (5.8 g, 25 mmol) and potassium carbonate (4.1 g, 30 mmol) was heated at 120° C. for 18 h, then cooled to room temperature and concentrated by rotary evaporation. The residue was dissolved in ethyl acetate (200 mL) and the organic phase washed with water (3×100 mL) and brine (100 mL), then dried (MgSO4), filtered and concentrated by rotary evaporation. The crude product was purified by column chromatography, eluting with ethyl acetate/cyclohexane (20/80, v/v). Selected fractions containing the product were concentrated via rotary evaporation to give 3.4 g (59%) of a red solid (m.p. 148° C.)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07101896B2 |
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| 出典データセット | uspto-grants-2006_09 |
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| ORD ID | ord-3c5af9c391014883b283a8713acbd156 |
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| 出典メモ | uspto-grants-2006_09 |
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