関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | tert-Butyldiphenylchlorosilane | HCID 94078 | — |
| 反応物 | 3-Hydroxy-3-(pyridin-4-yl)propanenitrile | HCID 21973939 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-(t-Butyldiphenylsiloxy)-3-(4-pyridyl)propionitrile | HCID 21974219 | 98.9% |
反応手順
Next, imidazole (4.60 g, 67.5 mmol) and N,N-dimethylformamide (30 ml) were added to the obtained 3-hydroxy-3-(4-pyridyl)propionitrile (1.00 g, 6.75 mmol), and the mixture was stirred at room temperature. t-Butyldiphenylchlorosilane (2.23 g, 8.10 mmol) was added to the mixture, and the whole was stirred for one day and then stirred further at an external temperature of 50° C. for three hours. Ethyl acetate (50 ml) and ether (50 ml) were added thereto, and the whole was washed with water (20 ml) three times and saturated brine (30 ml) successively. The organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give 3-(t-butyldiphenylsiloxy)-3-(4-pyridyl)propionitrile (2.58 g, 98.9%) as a colorless oily matter.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07741346B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-1afb9fe9375140518b7d7d258c08a4b4 |
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| 出典メモ | uspto-grants-2010_06 |
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