関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Dimethoxymethane | HCID 8020 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 3-Fluoro-4-nitrophenol | HCID 520948 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-Fluoro-4-(methoxymethoxy)-1-nitrobenzene | HCID 19932400 | 31.1% |
反応手順
A solution of 3-fluoro-4-nitrophenol (10.0 g, 0.064 mol), dimethoxymethane (19.3 g, 0.255 mol) and N,N-dimethylformamide (6.0 g, 0.083 mol) in toluene is heated to 65° C., treated dropwise with phosphorus oxychloride (15.7 g, 0.102 mol), stirred at 90° C. for two hours, cooled to room temperature and poured into ice water which contains five mL of 50% sodium hydroxide solution. After the ice has melted, the mixture is extracted with ether. The organic extract is washed with brine, dried over anhydrous sodium sulfate and concentrated in vacuo to give the title product as a yellow liquid (4.0 g) which is identified by 1HNMR spectral analysis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05424280 |
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| 出典データセット | uspto-grants-1995_06 |
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| ORD ID | ord-3714eea096134c3692e42ae9854125cb |
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| 出典メモ | uspto-grants-1995_06 |
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