関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Butyl bromide | HCID 8002 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2,3-Difluorophenol | HCID 80879 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Heptane | HCID 8900 | — |
| 生成物 | 1-Butoxy-2,3-Difluorobenzene | HCID 2782939 | 79.9% |
反応手順
2,3-Difluorophenol (21) (100.0 g) and sodium hydroxide (NaOH; 36.9 g) were added to water (300 ml) under a nitrogen atmosphere, and the stirring was continued at 70° C. 1-Bromobutane (158.0 g) was added thereto, and the stirring was continued at 70° C. for 2 hours. The reaction mixture obtained was cooled to 30° C., heptane (100 ml) and water (100 ml) were added, and mixed. The mixture was then allowed to separate into organic and aqueous phases. The extraction into an organic phase was carried out. The organic phase obtained was washed with brine and dried over anhydrous magnesium sulfate. Then, fractional distillation was carried out under reduced pressure, giving 114.4 g of 4-butoxy-2,3-difluorobenzene (22). The compound (22) obtained was a colorless oil having a boiling point of 109° C. to 110° C./20 mmHg. The yield based on the compound (21) was 80.0%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08216489B2 |
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| 出典データセット | uspto-grants-2012_07 |
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| ORD ID | ord-5505fad798d240c99a94a469200847b5 |
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| 出典メモ | uspto-grants-2012_07 |
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