関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Benzonitrile, 4-bromo- | HCID 12162 | — |
| 反応物 | (6-Fluoropyridin-3-yl)boronic acid | HCID 2783397 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 4-(6-Fluoropyridin-3-yl)benzonitrile | HCID 23115991 | 78% |
反応手順
A mixture of 4-bromobenzonitrile (0.20 g, 1.1 mmol), (6-fluoropyridin-3-yl)boronic acid (0.15 g, 1.1 mmol), [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II)dichloromethane (1:1) complex (0.04 g, 0.05 mmol) and potassium carbonate (0.46 g, 3.3 mmol) in 1,4-dioxane (7 mL), and water (3 mL) was heated at 110° C. for 2 h. After cooled to r.t., the mixture was diluted with MeOH, filtered, concentrated under reduced pressure and purified by flash chromatography on a silica gel column eluting with 5% MeOH in DCM to afford the desired product (0.17 g, yield: 78%). Analytic LCMS (M+H)+: m/z=199.2.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08481732B2 |
|---|
| 出典データセット | uspto-grants-2013_07 |
|---|
| ORD ID | ord-dedfe38c20a048b2b5132e59a29cbaa0 |
|---|
| 出典メモ | uspto-grants-2013_07 |
|---|
