関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,6-Lutidine | HCID 7937 | — |
| 反応物 | 3,5-Dichlorophenol | HCID 11571 | — |
| 反応物 | Triisopropylsilyl trifluoromethanesulfonate | HCID 2724529 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | (3,5-Dichlorophenoxy)tris(propan-2-YL)silane | HCID 21594466 | 91.3% |
反応手順
To a solution of 3,5-dichloro-phenol (5.9 g, 36 mmol) in methylene chloride (50 mL,) was added 2,6-lutidine (8.38 mL, 72.4 mmol) and triisopropylsilyl triflate (9.7 mL, 36 mmol) at 0° C. The resulting mixture was stirred at 0° C. for 4 h. The reaction was quenched with 0.1 N HCl and diluted with ethyl acetate. The organic solution was washed with brine, dried over Na2SO4 and concentrated in vacuo. The residue was purified with flash chromatography (5% ethyl acetate/hexanes) to give the desired product as a colorless oil (10.5 g, 91%). 1H NMR (400 MHz, CDCl3): δ 6.95 (t, J=1.8 Hz, 1 H), 6.76 (d, J=1.8 Hz, 2 H), 1.26 (m, 3 H), 1.09 (d, J=7.0 Hz, 18 H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08835423B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-1d1d219f150d49b980fe0b4cfd8300ce |
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| 出典メモ | uspto-grants-2014_09 |
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