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Water → 4-Bromo-3'-Fluoro-3-Methoxy-1,1'-Biphenyl
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 反応物 | 3-Fluorophenylboronic acid | HCID 2733986 | — |
| 反応物 | 1-Bromo-4-iodo-2-methoxybenzene | HCID 12187202 | — |
| 触媒 | HCID 178418807 | HCID 178418807 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 4-Bromo-3'-Fluoro-3-Methoxy-1,1'-Biphenyl | HCID 89762084 | — |
反応手順
A solution of PdCl2(dppf)-CH2Cl2 adduct (0.065 g, 0.080 mmol), 1-bromo-4-iodo-2-methoxybenzene (CombiBlocks, 0.250 g, 0.799 mmol), 3-fluorophenylboronic acid (0.123 g, 0.879 mmol) and potassium phosphate (0.848 g, 3.99 mmol) in dioxane (2.130 ml)/water (1.065 ml) was heated to 90° C. overnight. The reaction was diluted with DCM and separated from the aqueous via phase separator (Radleys Discovery Technologies). After concentration in vacuo, the material was purified via MPLC (12-g Redi Sep Gold), eluting with 0-100% ethyl acetate in heptanes to yield, after concentration, 4-bromo-3′-fluoro-3-methoxy-1,1′-biphenyl as an orange oil, which was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09346798B2 |
| 出典データセット | uspto-grants-2016_05 |
| ORD ID | ord-a2cb8c1e3c1c4b5f8dc08dffba635e8a |
| 出典メモ | uspto-grants-2016_05 |