関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Fluorobenzamide | HCID 71572 | — |
| 反応物 | Ethyl 4-bromo-3-oxopentanoate | HCID 12780443 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Ethyl[2-(4-fluorophenyl)-5-methyl-1,3-oxazol-4-yl]acetate | HCID 85817159 | 48.2% |
反応手順
A suspension of 4fluorobenzamide (12.9 g) and ethyl 4bromo-3-oxopentanoate (Chem Abs No. 3618769-6; 5.24 g) in anhydrous toluene (120 ml) was heated at 140° C. for 19 h, using a Dean-Stark trap. The solution was allowed to cool, filtered, and the residual solid washed with toluene (30 ml). The combined filtrate and washings were concentrated in vacuo to give a brown oil, which was purified by Biotage flash chromatography on silica gel (90 g column), eluting with ethyl acetate:cyclohexane (5:95, 7.5:92.5, 10:90), to give the title compound as a yellow solid (2.98 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07560548B2 |
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| 出典データセット | uspto-grants-2009_07 |
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| ORD ID | ord-4a4170c5aeee4106806b662e8d978de3 |
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| 出典メモ | uspto-grants-2009_07 |
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