関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | Thiodiglycol | HCID 5447 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | tert-Butyldiphenylchlorosilane | HCID 94078 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-[2-(t-Butyldiphenylsilyloxy)ethylthio]ethanol | HCID 59750807 | 54.2% |
反応手順
In dichloromethane (200 ml) were dissolved 2,2′-thiodiethanol (10.0 g, 81.8 mmol) and imidazole (4.70 g, 69.0 mmol), followed by the dropwise addition of t-butylchlorodiphenylsilane (15.0 ml, 57.7 mmol) at room temperature. After completion of the dropwise addition, the reaction mixture was stirred at room temperature for 14 hours. After concentration under reduced pressure, diethyl ether was added to the residue. Then, the insoluble matter was filtered off. The residue obtained by concentrating the filtrate under reduced pressure was subjected to flash silica gel chromatography, and the fraction obtained from the hexane:ethyl acetate=3:1 eluate was concentrated under reduced pressure, whereby the title compound (11.3 g, 31.3 mmol, 54%) was obtained as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07399775B2 |
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| 出典データセット | uspto-grants-2008_07 |
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| ORD ID | ord-b676ef213e204279a50daff62ebef92f |
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| 出典メモ | uspto-grants-2008_07 |
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