反応式
Br[C:2]1[N:3]([CH2:9][O:10][CH2:11][CH2:12][Si:13]([CH3:16])([CH3:15])[CH3:14])[C:4]([Br:8])=[C:5]([Br:7])[N:6]=1.[NH:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1>>[Br:7][C:5]1[N:6]=[C:2]([N:17]2[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]2)[N:3]([CH2:9][O:10][CH2:11][CH2:12][Si:13]([CH3:16])([CH3:15])[CH3:14])[C:4]=1[Br:8]参加物
3
実験手順
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:
後処理
- customwas irradiated at 130° C. for 15 min in a microwave reactor
- customThe reaction mixture was partitioned between DCM and water (100 mL, 1/1)
- customThe layers were separated
- extractionthe aqueous layer was extracted with DCM (2×50 mL)
- dry with materialThe combined organic layers were dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe resulting was purified by flash chromatography (SiO2, 100:0-90:10 DCM-MeOH)
出典と根拠
- ORDレコード
- ord-61ceab9ef5cb4903aae47a2eeeb0631c
- 出典データセット
- uspto-grants-2014_10
- 特許番号
- US08865732B2
関連ノート
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