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3-Hydroxybenzaldehyde → 3-(t-Butyldimethylsilyloxy)benzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Hydroxybenzaldehyde | HCID 101 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-(t-Butyldimethylsilyloxy)benzaldehyde | HCID 11207111 | — |
反応手順
3-Hydroxybenzaldehyde (5.0 g, 40.9 mmol) was dissolved in acetonitrile (10.0 mL). Subsequently, potassium carbonate (11.3 g, 81.9 mmol), and then tert-butyldimethylchlorosilane (7.4 g, 49.1 mmol) were added thereto, and the resultant mixture was stirred at room temperature. After completion of reaction, ethyl acetate was added thereto, followed by washing sequentially with water and brine, and drying over anhydrous sodium sulfate. The reaction mixture was subjected to filtration, concentration under reduced pressure, and purification by silica gel column chromatography (n-hexane/ethyl acetate=20/1), whereby the target compound was obtained (9.1 g, 94%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07183295B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-bf7cce1f6f964bab81c4ef86d74f3c34 |
| 出典メモ | uspto-grants-2007_02 |