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Imidazole → ({4'-Bromo-[1,1'-biphenyl]-4-yl}oxy)(tert-butyl)dimethylsilane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| 反応物 | 4-Bromo-4'-hydroxybiphenyl | HCID 95093 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | ({4'-Bromo-[1,1'-biphenyl]-4-yl}oxy)(tert-butyl)dimethylsilane | HCID 3765121 | 88.1% |
反応手順
tert-Butyldimethylsilyl chloride (1.8 g) was added over 30 minutes to a stirred solution of 4-bromo-4'-hydroxybiphenyl (2.49 g) and imidazole (1.63 g) in dimethylformamide (15 ml) whilst keeping the temperature of the reaction mixture below 10° C. The reaction mixture was stirred at room temperature for 18 hours. Diethyl ether (225 ml) was added, the ether washed with saturated sodium hydrogen carbonate solution (3×60 ml) and brine (100 ml), dried (MgSO4) and evaporated to yield, as a colourless oil, 4-bromo-4'-(tert-butyldimethylsilyloxy)biphenyl (3.2 g); NMR (CDCl3): 0.2(6H, s), 1.0(9H, s), 6.8-6.9(2H, d), 7.3-7. 4(4H, m) and 7.45-7.55(2H, d).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05792777 |
| 出典データセット | uspto-grants-1998_08 |
| ORD ID | ord-b0990df56b714f7a96ecf25dd8db54d2 |
| 出典メモ | uspto-grants-1998_08 |