関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Phenoxybenzyl chloride | HCID 93291 | — |
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 触媒 | Hexadecyltributylphosphonium bromide | HCID 84716 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 13194582 | HCID 13194582 | 49% |
反応手順
3-Phenoxybenzyl chloride (4.37 g), potassium fluoride (5.8 g), tri-n-butylhexadecylphosphonium bromide (1.2 g) and water (10 ml) were stirred for a period of 8 hours in a pressure bottle heated at a temperature of 130° C. The oil was separated and the aqueous phase was diluted with water and extracted with ethylene dichloride. The oil and ethylene dichloride extract were combined and the phosphonium salt was removed by chromatography over silica gel (15 g). The eluate was concentrated and distilled to give 3-phenoxybenzyl fluoride (1.96 g; 49%) b.p. 92°-95° C. at 0.3 mm Hg. (The product was stabilized by the addition of a small amount of anhydrous calcium carbonate to prevent acid catalysed polymerization).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04376784 |
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| 出典データセット | uspto-grants-1983_03 |
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| ORD ID | ord-cdcd3a4ab5264453a0fe4d4efc250155 |
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| 出典メモ | uspto-grants-1983_03 |
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