関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Bromodiphenyl Ether | HCID 7565 | — |
| 反応物 | Isopropenyl acetate | HCID 7916 | — |
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 反応物 | Methoxytri-n-butylstannane | HCID 11964040 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-(4-Phenoxyphenyl)propan-2-one | HCID 19591523 | 83% |
反応手順
75.0 g of 4-bromodiphenyl ether, 129 ml of tributyltin methoxide, 45.0 g of isopropenyl acetate and 2,47 g of dichlorobis{tri(o-tolyl)phosphine}palladium, were dissolved in 300 ml of toluene and refluxed under heating for 3 hours. The reaction solution was left to cool to room temperature, and then, a saturated potassium fluoride aqueous solution was added, followed by stirring for one hour. Then, the product was subjected to celite filtration and washed with ethyl acetate. The filtrate and washing liquid were put together. Then, the organic layer was separated and washed with a saturated sodium chloride aqueous solution and then dried over anhydrous magnesium sulfate. The drying agent was filtered off, and then, the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=15/1→10/1) to obtain 56.3 g (yield: 83%) of the above identified compound as yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06011174 |
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| 出典データセット | uspto-grants-2000_01 |
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| ORD ID | ord-16f48f99f052458ab881bcbd42a77a81 |
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| 出典メモ | uspto-grants-2000_01 |
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