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Water → 2-(2,4-Difluorophenoxy)-1-(4-(naphthalen-2-ylsulfonyl)piperazin-1-yl)ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,4-Difluorophenol | HCID 123051 | — |
| 反応物 | 2-Chloro-1-[4-(naphthalene-2-sulfonyl)piperazin-1-yl]ethan-1-one | HCID 2405875 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-(2,4-Difluorophenoxy)-1-(4-(naphthalen-2-ylsulfonyl)piperazin-1-yl)ethanone | HCID 40113484 | 73.87% |
反応手順
2,4-difluoro phenol (110 mg, 0.85 mmol), 2-chloro-1-(4-(naphthalen-2-ylsulfonyl)piperazin-1-yl)ethanone (compound 5, 0.3 g, 0.85 mmol) and anhydrous potassium carbonate (0.352 g, 2.55 mmol) were stirred for over night in dry acetonitrile (20 mL). The mixture was poured into a large volume of water and the solution extracted with ether. Un-reacted phenol was removed with cold 1N NaOH solution. The ether extract was dried over anhydrous sodium sulphate, filtered and concentrated under reduced pressure. The crude material was purified by re-crystallization to yield the title compound (280 mg, 73.87% yield) as an off-white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09115086B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-2ace2b203cc049328bed182f1811f1cb |
| 出典メモ | uspto-grants-2015_08 |