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Sodium Bicarbonate → 8-(4-(4-Methoxyphenyl)-5-(p-tolyl)thiazol-2-yl)-1,4-dioxaspiro[4.5]decane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 2-Bromo-1-(4-methoxyphenyl)-2-(p-tolyl)ethanone | HCID 46398776 | — |
| 反応物 | 1,4-Dioxaspiro[4.5]decane-8-carbothioamide | HCID 57929925 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 8-(4-(4-Methoxyphenyl)-5-(p-tolyl)thiazol-2-yl)-1,4-dioxaspiro[4.5]decane | HCID 67296392 | 81% |
反応手順
A solution of 1,4-dioxaspiro[4.5]decane-8-carbothioamide (Reference Example 94) (389 mg, 1.93 mmol) and 2-bromo-1-(4-methoxyphenyl)-2-(p-tolyl)ethanone (588 mg, 1.84 mmol) in acetonitrile (9.2 mL) was stirred at room temperature for 4 hours. Saturated aqueous sodium hydrogen carbonate solution was added to the reaction solution, and the resulting solution was extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by flash chromatography (silica gel, n-hexane/ethyl acetate) to obtain the captioned compound (630 mg, 1.49 mmol, 81%) as a colorless amorphous product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08247569B2 |
| 出典データセット | uspto-grants-2012_08 |
| ORD ID | ord-0333eb0cc5ee4d47b94de08d125eb4dd |
| 出典メモ | uspto-grants-2012_08 |