関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | Dimercaprol | HCID 3080 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-t-BUTYLDIMETHYLSILYLOXY-2,3-DIMERCAPTOPROPANE | HCID 21255839 | 94.6% |
反応手順
To a solution of 2,3-dimercapto-1-propanol (15.0 ml, 150 mmol) and imidazole (15.3 g, 224 mmol, 1.5 eq) in THF (300 mL) was added t-butyldimethylsilyl chloride (21.4 g, 142 mmol, 0.95 eq) at 0° C. The mixture was stirred at 0° C. for 1 hr and at room temperature for 18 hr. A saturated solution of ammonium chloride was added and the aqueous phase was extracted with dichloromethane. The organic layer was dried with anhydrous sodium sulphate and the solvent was evaporated under reduced pressure. The crude material was purified by flash chromatography with a mixture of hexane and ethyl acetate (90:10) to give the pure compound (32.04 g) in 94.5% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05955610 |
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| 出典データセット | uspto-grants-1999_09 |
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| ORD ID | ord-4c630c3fba9043b79c5c1a3b2632f55d |
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| 出典メモ | uspto-grants-1999_09 |
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