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3-Hydroxybenzyl alcohol → 3-((((1,1-Dimethylethyl)dimethylsilyl)oxy)methyl)phenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Hydroxybenzyl alcohol | HCID 102 | — |
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-((((1,1-Dimethylethyl)dimethylsilyl)oxy)methyl)phenol | HCID 14940556 | 92.3% |
反応手順
To a solution of 79 g of 3-(hydroxymethyl)phenol in 300 mL of DMF cooled at 0° C. was added 50 g of imidazole followed by 101 g of tert-butyl(chloro)dimethylsilane. The reaction was warmed to rt and stirred overnight. The reaction was quenched with aqueous NH4Cl, extracted with EtOAc and washed with brine, dried over sodium sulfate, evaporated, and purified by flash chromatography (10–30% EtOAc/hexane) to afford 140 g of the title compound as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07199154B2 |
| 出典データセット | uspto-grants-2007_04 |
| ORD ID | ord-aee082bad9f3440dbf63d25c9da2ab45 |
| 出典メモ | uspto-grants-2007_04 |