関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Ethyl 2-butynoate | HCID 78043 | — |
| 反応物 | 1,3-Benzoxazol-4-ol | HCID 13720697 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (E)-3-(benzooxazol-4-yloxy)-but-2-enoic acid ethyl ester | HCID 66895566 | 100.1% |
反応手順
A stirred mixture of benzooxazol-4-ol (0.388 g, 2.87 mmol), ethyl-2-butynoate (1.93 g, 17.2 mmol) a catalytic amount of 4-dimethylaminopyridine and potassium carbonate (0.595 g, 4.30 mmol) in tetrahydrofuran (20 mL) was placed in a sealed tube and heated at 80° C. for 2 h. The reaction mixture was filtered and the filtrate was collected and concentrated in vacuo. The resulting residue was purified by ISCO column chromatography (Silicycle 40 g, 2% to 15% ethyl acetate/hexanes) which afforded (E)-3-(benzooxazol-4-yloxy)-but-2-enoic acid ethyl ester (710 mg, 100%) as a light yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07741327B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-a6e7976868214a29b3b7aa30f68365d0 |
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| 出典メモ | uspto-grants-2010_06 |
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