関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-(Methoxymethyl)-2-nitrobenzene | HCID 12616689 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2-(Methoxymethyl)aniline | HCID 12334306 | 101.8% |
反応手順
528 g of 21.8% strength Na2 [Fe(CO)4 ] solution (0.6 mol; 1 kg of the solution contains 633 g of water, 218 g of Na2 [Fe(CO)4 ], 108 g of Na2CO3 and 41 g of NaOH) are added dropwise to 101 g (0.6 mol) of o-methoxymethylnitrobenzene (Example 3a) in 1 l of methanol at 20°-30° C. Stirring is carried out for 1 hour at room temperature, after which the reaction mixture is diluted with ether. A brown oil separates out in the reaction vessel. The total reaction mixture is poured onto a silica gel column and is eluted with ether. Thereafter, the ether phase is evaporated, the residue is taken up in methylene chloride and the solution is dried over MgSO4. It is filtered under suction over silica gel and the solvent is then evaporated off under reduced pressure. The residue is purified by column chromatography with hexane and methylene chloride. 83.8 g of o-methoxymethylaniline are obtained as a brown oil, which is directly reacted further.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05824705 |
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| 出典データセット | uspto-grants-1998_10 |
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| ORD ID | ord-6c69e0ce99d441449627f86473f8a618 |
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| 出典メモ | uspto-grants-1998_10 |
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