참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Phosphonic acid, dimethyl ester | HCID 13361 | — |
| 반응물 | 1-(4-fluoro-phenyl)-2-methyl-1H-imidazole-4-carbaldehyde | HCID 85997993 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | 4-Ethynyl-1-(4-fluorophenyl)-2-methyl-1H-imidazole | HCID 11665595 | — |
반응 단계
Diazo-2-oxo-propyl)-phosphonic acid dimethyl ester (6.51 g, 33.9 mmol) was dissolved in 100 mL methanol. Potassium carbonate (7.81 g, 56.5 mmol) was added. A solution of 1-(4-fluoro-phenyl)-2-methyl-1H-imidazole-4-carbaldehyde (5.77 g, 45 mmol) in 100 mmol methanol was added dropwise at room temperature. The reaction mixture was stirred at room temperature overnight. The solvent was evaporated. The residue was taken up in 150 mL water and extracted three times with ethyl acetate (150 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 100:0->0:100 gradient) and the desired compound was obtained as a white solid (3.81 g, 67%), MS: m/e=200.1 (M+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08481548B2 |
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| 출처 데이터셋 | uspto-grants-2013_07 |
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| ORD ID | ord-99961545464642ebb8da4b13f6b117db |
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| 출처 메모 | uspto-grants-2013_07 |
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