関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Nitrophenethyl bromide | HCID 79266 | — |
| 反応物 | 2-methyl-4,4-diphenyl-1H-imidazol-5-one | HCID 619503 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 2-Methyl-3-[2-(4-nitro-phenyl)-ethyl]-5,5-diphenyl-3,5-dihydro-imidazol-4-one | HCID 68466653 | 46.9% |
反応手順
2-Methyl-5,5-diphenyl-3,5-dihydro-imidazol-4-one (1 g, 4 mmol) and 1-(2-bromo-ethyl)-4-nitro-benzene (919 mg, 4 mmol) and potassium carbonate (669 mg, 4.8 mmol) are dissolved in 12 mL acetone and the reaction mixture is heated at 70° C. for 5 min in the microwave oven (Biotage Initiator) and again heated for 5 min at 120° C. The mixture is cooled to room temperature, filtered and the filtrate evaporated to yield the crude product which is subjected to flash chromatography. ISCO Companion CombiFlash, 80 g silica gel, cyclohexane/ethyl acetate, followed by a second purification step, 40 g silica gel, acetone/cylohexane to yield 2-methyl-3-[2-(4-nitro-phenyl)-ethyl]-5,5-diphenyl-3,5-dihydro-imidazol-4-one (750 mg, 45%). LC/MS at 254 nm; [M+H] 400; Rt 3.391 min.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07786155B2 |
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| 出典データセット | uspto-grants-2010_08 |
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| ORD ID | ord-71e545d6397c40efb131e2111786c2ee |
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| 出典メモ | uspto-grants-2010_08 |
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