関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phenol | HCID 996 | — |
| 反応物 | Diisopropyl Ether | HCID 7914 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 4-Chloro-2-(dimethoxymethyl)-1-nitrobenzene | HCID 3570093 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | 2-(Dimethoxymethyl)-1-nitro-4-phenoxybenzene | HCID 3480452 | — |
反応手順
A mixture of 4-chloro-2-dimethoxymethyl-1-nitrobenzene (11.55 g, 0.0500 mol), phenol (4.70 g, 0.0500 mol), and potassium carbonate (8.16 g, 0.0600 mol) in DMA (100 mL) was stirred at 150° C. for 6 h. After cooling, the reaction mixture was poured into water and treated with diisopropyl ether. The organic layer was separated, washed with 10% aqueous KOH solution, dried (MgSO4), filtered, and concentrated. The resulting residue was purified by column chromatography on silica gel using as eluent CH2Cl2:petroleum ether (40:60, 60:40, 100:0 gradient). The product containing fractions were combined and evaporated to yield a residue which was dissolved in CH2Cl2 and washed with 10% aqueous KOH solution to remove the remaining phenol. Drying and evaporation yielded a residue.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08383637B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-1bdecdc5e01d40cdb0b37d0f40d60b20 |
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| 出典メモ | uspto-grants-2013_02 |
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