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Imidazole → HCID 178455374、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| 反応物 | HCID 178521634 | HCID 178521634 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178455374 | HCID 178455374 | — |
反応手順
To a solution of cis-3-benzyloxymethylcyclobutanol (Albany Molecular Research Institute, 1.0 g, 5.2 mmol) in 50 mL of CH2Cl2 was added imidazole (2.7 g, 39 mmol) followed by tert-butyldimethylsilyl chloride (3.9 g, 26 mmol). This mixture stirred at ambient temperature for 2 hours and was quenched with 10 mL of saturated aqueous NH4Cl. The layers were separated and the aqueous layer was extracted with three 5 mL of portions of CH2Cl2. The combined organic extracts were dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure. Purification via column chromatography (SiO2, 75% hexanes in ethyl acetate) afforded the title compound. MS (DCI/NH3) m/z 307 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08546583B2 |
| 出典データセット | uspto-grants-2013_10 |
| ORD ID | ord-ba51fc323a2b4dbe951cc6d494e1fa75 |
| 出典メモ | uspto-grants-2013_10 |