関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-(4-Fluorophenyl)ethanol | HCID 73946 | — |
| 反応物 | Bromotrimethylsilane | HCID 76113 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(1-Bromoethyl)-4-fluorobenzene | HCID 13389030 | — |
反応手順
0.5 g of 1-(4-fluorophenyl)ethanol is dissolved in 20 cm3 of dichloromethane, under an inert atmosphere, at a temperature close to 20° C. 1.24 cm3 of pure bromo(trimethyl)silane are introduced in two lots to the reaction mixture. The latter is stirred at a temperature close to 20° C. for 48 h, then it is washed with a saturated aqueous solution of sodium chloride, dried over a phase separation cartridge and concentrated using a rotary evaporator under reduced pressure (5 kPa). The 700 mg of crude product obtained are purified by filtration through a silica pellet (eluent: 10% ethyl acetate/90% cyclohexane). After concentrating the fractions under reduced pressure, 439 mg of 1-(1-bromoethyl)-4-fluorobenzene are obtained in the form of a colorless thick oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08372864B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-45567561ff1c4ecf9cfba6aac71202f4 |
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| 出典メモ | uspto-grants-2013_02 |
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