関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Aluminum iodide | HCID 82222 | — |
| 反応物 | 3-(3,5-Dimethoxyphenyl)-1-propene | HCID 524874 | — |
| 溶媒 | Carbon Disulfide | HCID 6348 | — |
| 生成物 | 5-Allylbenzene-1,3-diol | HCID 639188 | — |
反応手順
The Pd-catalyzed cross-coupling reaction of 5-Bromo-1,3-dimethoxybenzene with allyl boronic acid pinacol ester produced 5-allyl-1,3-dimethoxybenzene 1 in excellent yield. AlI3 will be used for demethylating 5-Allyl-1,3-dimethoxybenzene with CS2 as solvent to produce 5-allylresorcinol 2. The bis(phosphinite) PCP ligands 3 will be obtained by diphosphorylation of 5-allylresorcinol 2 with the respective chlorophosphine and sodium hydride as a base. Iridium complexes 4 will be obtained from reaction of the respective PCP ligands 3 with [Ir(COD)Cl]2 or [Ir(COE)2Cl]2. Hydrosilylation of complexes 4 will produce the hydrosilylated complexes 5. Reaction of complexes 5 with silica gel will afford the Si2O-supported Ir complexes 6. To date, 5-allyl-1,3-dimethoxybenzene 1 has been prepared in 92% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07902417B2 |
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| 出典データセット | uspto-grants-2011_03 |
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| ORD ID | ord-c2d1826b42a845f696bf59f6d9185409 |
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| 出典メモ | uspto-grants-2011_03 |
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