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Pyridine, hydrofluoride (1:1) → 4-(2-Fluoro-1,2-dimethylpropyl)-2-methyl-1-trityl-1h-imidazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine, hydrofluoride (1:1) | HCID 64774 | — |
| 反応物 | 1-(Trimethylsilyl)ethanol | HCID 12447898 | — |
| 反応物 | 2,2-dimethyl-1-(2-methyl-1-trityl-1H-imidazol-4-yl)propan-1-ol | HCID 68668143 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(2-Fluoro-1,2-dimethylpropyl)-2-methyl-1-trityl-1h-imidazole | HCID 59161985 | — |
反応手順
2,2-Dimethyl-1-(2-methyl-1-trityl-1H-imidazol-4-yl)propan-1-ol (200 mg, 0.49 mmol) in a minimal volume of methylene chloride was added to HF-pyridine (2 mL) at 0° C. After stirring at ambient temperature overnight, the reaction was added dropwise to TMS-ethanol and partitioned between ethyl acetate and saturated aqueous sodium bicarbonate. Organic phase was washed with brine, dried (sodium sulfate) and concentrated in vacuo. Chromatography over silica eluting with 10-70% ethyl acetate/hexane afforded the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08193228B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-b7aae145552f46dca8e008e9f0d81512 |
| 出典メモ | uspto-grants-2012_06 |