関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Benzonitrile, m-chloro- | HCID 13015 | — |
| 反応物 | HCID 178418573 | HCID 178418573 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-(3-Chlorophenyl)ethanone | HCID 14933 | — |
反応手順
Under a nitrogen atmosphere, 36.7 mL (0.11 mole) of methylmagnesium bromide (3.0M in diethyl ether) is stirred, and a solution of 13.8 grams (0.10 mole) of 3-chlorobenzonitrile in 50 mL of dry tetrahydrofuran is added slowly dropwise. Upon completion of addition, the reaction mixture is warmed to reflux where it is stirred for about 18 hours. After this time the reaction mixture is cooled to ambient temperature, and about 40 mL of methanol is added dropwise. Upon completion of addition, the reaction mixture is stirred for two hours and then filtered. The filtrate is then stirred for about 18 hours with 35 grams of silica gel and 100 mL of water. The mixture is filtered, and the filtrate is diluted with ethyl acetate. The mixture is then washed with water, and the organic layer is dried with magnesium sulfate. The mixture is filtered, and the filtrate is concentrated under reduced pressure, yielding methyl 3-chlorophenyl ketone.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05712281 |
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| 出典データセット | uspto-grants-1998_01 |
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| ORD ID | ord-1518c00294774bacbe3ba301d4199895 |
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| 出典メモ | uspto-grants-1998_01 |
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