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Sodium Carbonate → 3,5-Dipyrenylbromobenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 1,2,3-Tribromobenzene | HCID 11842 | — |
| 反応物 | Pyren-1-ylboronic acid | HCID 5084102 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3,5-Dipyrenylbromobenzene | HCID 71424737 | 38.6% |
反応手順
Under the atmosphere of argon gas, 6 g of tribromobenzene available as a commercial reagent, 9.4 g of 1-pyrenyl boronic acid and 0.88 g of tetrakis(triphenylphophine)palladium were dissolved in 150 ml of toluene, and then the 57 ml of 2M sodium carbonate aqueous solution was added therein, followed by 7 hours reflux on heating. After standing to cool, the precipitated solid was separated through filtration, and then followed by washing with water and methanol, and drying. The obtained solid was refined through a silica gel chromatography (developing solvent: toluene/hexane=1/3) and then 4.1 g of 3,5-dipyrenylbromobenzene of pale yellow solid was obtained (Yield: 38%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07560604B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-8ca79cd2f7be4a7193007483ffae5a51 |
| 出典メモ | uspto-grants-2009_07 |