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Piperazine → 1-(4,5-Dibromo-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-imidazol-2-yl)piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Piperazine | HCID 4837 | — |
| 反応物 | 2,4,5-tribromo-1-[[2-(trimethylsilyl)ethoxy]methyl]-1H-Imidazole | HCID 10906203 | — |
| 生成物 | 1-(4,5-Dibromo-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-imidazol-2-yl)piperazine | HCID 58625831 | 28.2% |
反応手順
A mixture of 2,4,5-tribromo-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-imidazole (653 mg, 1.5 mmol) and piperazine (1.03 g, 12.0 mmol) under Ar was irradiated at 130° C. for 15 min in a microwave reactor. The reaction mixture was partitioned between DCM and water (100 mL, 1/1). The layers were separated and the aqueous layer was extracted with DCM (2×50 mL). The combined organic layers were dried (Na2SO4), filtered and concentrated in vacuo. The resulting was purified by flash chromatography (SiO2, 100:0-90:10 DCM-MeOH) to provide 186 mg of 1-(4,5-dibromo-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-imidazol-2-yl)piperazine as a colorless oil:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08865732B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-61ceab9ef5cb4903aae47a2eeeb0631c |
| 出典メモ | uspto-grants-2014_10 |