関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Lithium Bromide | HCID 82050 | — |
| 反応物 | 2-Bromo-1-(difluoromethoxy)-3-nitrobenzene | HCID 58100766 | — |
| 反応物 | HCID 178418546 | HCID 178418546 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Difluoromethoxy-6-nitrobenzonitrile | HCID 58100764 | 84.6% |
反応手順
A mixture of 2-bromo-1-difluoromethoxy-3-nitro-benzene (1 g, 3.7 mmol), CuCN (0.40 g, 4.5 mmol) and LiBr (0.32 g, 3.7 mmol) in tetrahydrofuran (10 ml) are heated in a microwave oven at 200° C. for 40 minutes. The reaction mixture is cooled to ambient temperature, diluted with toluene and washed with aqueous sodium bromide (1M) and aqueous sodium hydrogen sulfite (saturated). The organic phase is dried over sodium sulfate and concentrated. The residue is purified by HPLC to give 2-difluoromethoxy-6-nitrobenzonitrile (0.67 g, 84% yield). 1H-NMR (CDCl3, 400 MHz): 8.20 (d, 1H), 7.85 (t, 1H), 7.75 (d, 1H), 6.75 (t, 1H) ppm.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08524896B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-47972b48f6ac4d3da12438dc0306f2c1 |
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| 出典メモ | uspto-grants-2013_09 |
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