関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Propargyl alcohol | HCID 7859 | — |
| 反応物 | Dabco | HCID 9237 | — |
| 反応物 | Ethyl nitroacetate | HCID 69379 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl 5-(hydroxymethyl)isoxazole-3-carboxylate | HCID 8027233 | 81% |
反応手順
To a mixture of propargyl alcohol (1.0 mL; 16.76 mmol) and ethyl 2-nitroacetate (3.79 mL; 33.52 mmol) in ethanol (23.5 mL) in an Ace pressure tube was added 1,4-diazobicyclo[2.2.2]octane (DABCO, 0.194 g; 1.68 mmol). The tube was heated at 80° C. for 72 h. After cooling, the mixture was evaporated to dryness and the residue was purified by flash chromatography on silica gel (eluent: 0 to 6% methanol in dichloromethane) to yield 2.32 g (81%) of ethyl 5-(hydroxymethyl)isoxazole-3-carboxylate as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09434722B2 |
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| 出典データセット | uspto-grants-2016_09 |
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| ORD ID | ord-2f958587927640de86d953d3ffdfc723 |
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| 出典メモ | uspto-grants-2016_09 |
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