関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Ethyl trans-3-dimethylaminoacrylate | HCID 5369162 | — |
| 反応物 | N-cyclopropyl-2-chloro-2-hydroxyimino-acetamide | HCID 85344446 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-(Cyclopropylcarbamoyl)-isoxazole-4-carboxylic acid ethyl ester | HCID 70097900 | — |
反応手順
A mixture of N-cyclopropyl-2-chloro-2-hydroxyimino-acetamide (2 g, 12.3 mmol) and (E)-3-(dimethylamino)-acrylic acid ethyl ester (1.76 ml, 12.3 mmol) in THF (25 ml) was heated at 75° C. for 2 h. The reaction was then cooled to r.t., poured into 100 mL ethyl acetate and extracted with 1 M HCl. The aqueous layers were back-extracted with ethyl acetate. The organic phase was washed with water and brine, dried and evaporated. The product was obtained after purification by silica gel chromatography using a heptane/ethyl acetate gradient as light yellow solid (1.6 g, 58%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08703768B2 |
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| 出典データセット | uspto-grants-2014_04 |
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| ORD ID | ord-c0bc2d58bbb842d892b8d1461e1e93ad |
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| 出典メモ | uspto-grants-2014_04 |
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