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Imidazole → (3-((Tert-butyldimethylsilyloxy)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 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| 反応物 | 1,3-Benzenedimethanol | HCID 69374 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (3-((Tert-butyldimethylsilyloxy)methyl)phenyl)methanol | HCID 10658493 | 42.7% |
反応手順
33.3 g of tert-butyldimethylsilyl chloride is added to a solution of 30 g of 3-hydroxymethylbenzyl alcohol and 30 g of imidazole in 250 ml of dimethylformamide at 0° C. under argon and stirred for. 20 hours at 25° C. It is diluted with 1.5 1 of ether, shaken twice with 100 ml of 10% sulfuric acid each, washed neutral with brine, dried on sodium sulfate and concentrated by evaporation in a vacuum. The residue is chromatographed on silica gel. With hexane/0-80% ether, 23.4 g of 3-tert-butyldimethylsilyloxymethyl-benzyl alcohol is obtained as colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05614634 |
| 出典データセット | uspto-grants-1997_03 |
| ORD ID | ord-e754f00fe4c64286bc920a8d5febe93e |
| 出典メモ | uspto-grants-1997_03 |