関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Phosphonic acid, dimethyl ester | HCID 13361 | — |
| 反応物 | 1-Cyclopropyl-2,5-dimethyl-1H-imidazole-4-carbaldehyde | HCID 21985387 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1-cyclopropyl-4-ethynyl-2,5-dimethyl-1H-imidazole | HCID 21985385 | — |
反応手順
Diazo-2-oxo-propyl)-phosphonic acid dimethyl ester (0.6 g, 3 mmol) was dissolved in 10 mL of methanol. Potassium carbonate (0.74 g, 5 mmol) was added. A solution of 1-Cyclopropyl-2,5-dimethyl-1H-imidazole-4-carbaldehyde (0.42 g, 3 mmol) in 5 ml methanol was added drop wise at room temperature. The reaction mixture was stirred at room temperature overnight. The solvent was evaporated. The residue was taken up in 15 mL water and extracted three times with ethyl acetate (15 ml each). The combined organic extracts were dried with sodium sulfate, filtered and evaporated. The crude product was purified by flash chromatography on silica gel (heptane/ethyl acetate 80:20→0:100 gradient) and the desired compound was obtained as a white solid (0.12 g, 30%), MS: m/e=161.4 (M+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07091222B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-edc697d54b1148c0900b356e7c803263 |
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| 出典メモ | uspto-grants-2006_08 |
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