関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Ethyl nitroacetate | HCID 69379 | — |
| 反応物 | Cyclopentylacetylene | HCID 136725 | — |
| 触媒 | Dabco | HCID 9237 | — |
| 生成物 | Ethyl 5-(hydroxymethyl)isoxazole-3-carboxylate | HCID 8027233 | 96% |
反応手順
To a mixture of ethynylcyclopentane (0.74 mL; 6.05 mmol) and ethyl 2-nitroacetate (1.37 mL; 12.11 mmol) in ethanol (9 mL) in an Ace pressure tube was added 1,4-diazobicyclo[2.2.2]octane (DABCO, 0.070 g; 0.60 mmol). The tube was heated at 80° C. for 96 h. The mixture was evaporated. The flash chromatography on silica gel (eluent: 20 to 80% dichloromethane in heptane) of the residue provided 1.21 g (96%) 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-3e064e2a2ad34f739bdcb8230f179c09 |
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| 出典メモ | uspto-grants-2016_09 |
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