関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,3-Dibromobenzene | HCID 7927 | — |
| 反応物 | 3-Hydroxy-3-methyl-2-butanone | HCID 8261 | — |
| 反応物 | 1,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine) | HCID 636044 | — |
| 反応物 | sodium 2-methylpropan-2-olate | HCID 178418730 | — |
| 触媒 | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ammonium Chloride | HCID 25517 | — |
| 生成物 | 1-(3-Bromo-phenyl)-3-hydroxy-3-methyl-butan-2-one | HCID 69374151 | — |
反応手順
A mixture of 1,3-dibromobenzene (1.0 eq.), 3-hydroxy-3-methyl-butan-2-one (1.0 eq.), Pd2(dba)3 (0.02 eq.), xantphos (0.04 eq.) and t-BuONa (1.1 eq.) in THF (0.15M) was stirred at 60° C. for 2 h, poured in saturated aqueous NH4Cl and extracted with EtOAc (2×). The combined organic extracts were washed with brine, dried over Na2SO4, filtered and concentrated. Flash chromatography (Hex:EtOAc; 7:3) afforded the title compound as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07153968B2 |
|---|
| 出典データセット | uspto-grants-2006_12 |
|---|
| ORD ID | ord-341157c5382d465799e3515ab65a2bd0 |
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| 出典メモ | uspto-grants-2006_12 |
|---|
