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Diethyl Ether → 2-(4-Fluorophenyl)cyclohexan-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | 1-Bromo-4-fluorobenzene | HCID 9993 | — |
| 反応物 | 2-Chlorocyclohexanone | HCID 13203 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 2-(4-Fluorophenyl)cyclohexan-1-one | HCID 13089540 | — |
反応手順
The Grignard reagent prepared by adding 210 g of p-fluorobromobenzene in 800 ml. of anhydrous ether to 29.1 g of magnesium turnings in 50 ml. of ether was added, with cooling to keep the temperature of the reaction less than 15° C., to a solution of 158.4 g of 2-chlorocyclohexanone in 800 ml. of anhydrous benzene. The reaction was stirred at 25° for 18 hrs. then the ether was distilled off and the resulting benzene solution refluxed for 24 hrs. It was then poured into a mixture of 1 liter water and 200 ml. hydrochloric acid and extracted with ether. After evaporation of the ether the residue was distilled to yield 117 g (51%), b.p. 115 (0.2 mm). The material solidified on standing and was recrystallized from hexane, m.p. 56°-59° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04150135 |
| 出典データセット | uspto-grants-1979_04 |
| ORD ID | ord-cc94bd0bbb4b4af998b4594e7d673330 |
| 出典メモ | uspto-grants-1979_04 |