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Imidazole → (3-(((Tert-butyldiphenylsilyl)oxy)methyl)phenyl)methanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | 1,3-Benzenedimethanol | HCID 69374 | — |
| 反応物 | tert-Butyldiphenylchlorosilane | HCID 94078 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (3-(((Tert-butyldiphenylsilyl)oxy)methyl)phenyl)methanol | HCID 57049439 | — |
反応手順
To a solution of 1,3-phenylenedimethanol (10.00 g, 72.38 mmol, Aldrich) in DCM (200 mL) was added 1H-imidazole (5.17 g, 76.0 mmol, Aldrich), followed by the addition of tert-butylchlorodiphenylsilane (19.8 mL, 76.0 mmol, Aldrich) and 4-dimethylaminopyridine (0.88 g, 7.2 mmol, Aldrich). After stirring overnight, the reaction was partitioned between DCM and water, the organic layer was dried over sodium sulfate, filtered and concentrated. The product was purified by flash chromatography (gradient elution, 0 to 20% EtOAc/hexanes). Yield: (7.9 g, 29%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09309246B2 |
| 出典データセット | uspto-grants-2016_04 |
| ORD ID | ord-da68729bd8b14e24992ff15ebf72999b |
| 出典メモ | uspto-grants-2016_04 |