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tert-Butyldiphenylchlorosilane → 4-(tert-Butyldiphenylsilyloxymethyl)-1-(2-trimethylsilylethoxy methyl)-1H-imidazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | tert-Butyldiphenylchlorosilane | HCID 94078 | — |
| 反応物 | 1-(2-Trimethylsilylethoxymethyl)-1H-imidazole-4-methanol | HCID 69558376 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(tert-Butyldiphenylsilyloxymethyl)-1-(2-trimethylsilylethoxy methyl)-1H-imidazole | HCID 71087293 | — |
反応手順
1-(2-Trimethylsilylethoxymethyl)-1H-imidazole-4-methanol (100 g) was dissolved in dichloromethane (1 L), and under stirring TEA (122 mL), DMAP (5.35 g), and then TBDPSCl (149 mL) were added. After stirring for 1 day, the reaction mixture solution was washed with water, dried over anhydrous sodium sulfate, and subsequently the solvent was distilled off under reduced pressure. The resulting residue was purified by flash chromatography (ethyl acetate/hexane=25%-50%) using silica gel column (product name: Ultra Pack E, manufactured by Yamazen Corporation) to afford the title compound (146 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08653126B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-0740e4e2a6d74c7680fc97aab1e42bee |
| 出典メモ | uspto-grants-2014_02 |