関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 3-Methoxybenzonitrile | HCID 73712 | — |
| 反応物 | HCID 178418443 | HCID 178418443 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Methoxypropiophenone | HCID 10942788 | 99% |
反応手順
A solution of ethyl magnesium bromide in diethyl ether (58 ml, 3 M) was added dropwise at room temperature to a mixture of 3-methoxybenzonitrile (21.2 g, 0.159 mol) and dry THF (250 ml). When addition was complete the mixture was stirred for 1 h at room temperature, 3 h at 40° C. and finally stirred overnight at room temperature. Water (250 ml) was added followed by a saturated ammonium chloride solution (250 ml) and the mixture was stirred for 1 h at room temperature. The phases were separated and the aqueous phase was extracted with ethyl acetate (100 ml). The combined organic phases was dried (MgSO4) and the solvent evaporated in vacuo to give 25.9 g (99%) of 3-methoxypropiophenone.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06174898B1 |
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| 出典データセット | uspto-grants-2001_01 |
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| ORD ID | ord-a25213fbab6145e6a7bf02aef9f90f80 |
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| 出典メモ | uspto-grants-2001_01 |
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