関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Hydroquinone | HCID 785 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | (2-Bromoethoxy)-tert-butyldimethylsilane | HCID 3608067 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-[2-(Tert-butyl-dimethyl-silanyloxy)-ethoxy]-phenol | HCID 22033378 | — |
反応手順
To a stirred solution of hydroquinone (Aldrich, 11.01 g, 100 mmol) in DMF (300 mL), (2-bromo-ethoxy)-tert-butyl-dimethyl-silane (Aldrich, 12.0 g, 50 mmol), cesium carbonate (40.7 g, 125 mol) were added and the mixture was stirred at 60° C. overnight. The mixture was poured into water (300 mL) and 6N HCl was added to adjust the “pH” to 6. The mixture was extracted with EtOAc (3×60 mL) and the extracts were combined and dried. Removal of solvent gave the crude, which was chromatographied on a ISCO machine eluting with EtOAc/hexane (0-30%) to give a light brown solid. 5.71 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08134001B2 |
|---|
| 出典データセット | uspto-grants-2012_03 |
|---|
| ORD ID | ord-2448f86660f7407980735a152a45a52e |
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| 出典メモ | uspto-grants-2012_03 |
|---|
