関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | tert-Butyl methyl ether | HCID 15413 | — |
| 反応物 | [3-(Hydroxymethyl)phenyl]boronic acid | HCID 2734662 | — |
| 反応物 | 5-Bromo-2-iodopyrimidine | HCID 7006651 | — |
| 反応物 | Tripotassium phosphate trihydrate | HCID 18407952 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | (3-(5-Bromopyrimidin-2-yl)phenyl)methanol | HCID 59484879 | — |
反応手順
750 mg (0.65 mmol) of tetrakis(triphenylphosphine)palladium are added to a solution, kept under nitrogen, of 6.11 g (21.5 mmol) of 5-bromo-2-iodopyrimidine, 3.91 g (25.7 mmol) of 3-(hydroxymethyl)benzeneboronic acid and 9.11 g (42.9 mmol) of tripotassium phosphate trihydrate in 120 ml of dioxane and 14 ml of water, and the mixture is stirred at 90° C. for 18 hours. The reaction mixture is cooled to room temperature, tert-butyl methyl ether and water are added, and the mixture is filtered through kieselguhr. The organic phase of the filtrate is separated off, dried over sodium sulfate and evaporated. The residue is chromatographed on a silica-gel column with dichloromethane/methanol as eluent.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08431572B2 |
|---|
| 出典データセット | uspto-grants-2013_04 |
|---|
| ORD ID | ord-89e230f9231347cba7d7ab8110e549ea |
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| 出典メモ | uspto-grants-2013_04 |
|---|
