化工社化工社 化学情報印刷レポート · 研究参考用
Cesium carbonate → [2-(5-Chloro-2-fluoro-phenyl)-pyrido[2,3-d]pyrimidin-4-yl]-(3-fluoro-pyridin-4-yl)-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | Chlorimide | HCID 76939 | — |
| 反応物 | Binap, (A+-)- | HCID 634876 | — |
| 反応物 | 4-Amino-3-fluoropyridine | HCID 817122 | — |
| 反応物 | 4-Chloro-2-(5-chloro-2-fluoro-phenyl)-pyrido[2,3-d]pyrimidine | HCID 21113093 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | [2-(5-Chloro-2-fluoro-phenyl)-pyrido[2,3-d]pyrimidin-4-yl]-(3-fluoro-pyridin-4-yl)-amine | HCID 21113088 | 21.7% |
反応条件
| 温度 | 110 °C |
|---|
反応手順
To a suspension of dioxane (5 ml), Pd(OAc)2 (50 mg), BINAP (20 mg), 4-amino-3-fluoro-pyridine (42 mg) and Cs2CO3 (200 mg) was added the crude imino chloride, 4-Chloro-2-(5-Chloro-2-fluoro-phenyl)-pyrido[2,3-d]pyrimidine (100 mg, 0.34 mmol) in a sealed tube. The reaction mixture was heated to 110° C. for 15 h. The reaction mixture was cooled to r.t. and filtered through Celite® and the crude material was purified by silica gel flash column chromatography (95% to 5% gradient CH2Cl2/EtOAc) to afford [2-(5-Chloro-2 -fluoro-phenyl)-pyrido[2,3-d]pyrimidin-4-yl]-(3-fluoro-pyridin-4-yl)-amine (27.3 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07232824B2 |
| 出典データセット | uspto-grants-2007_06 |
| ORD ID | ord-f160a7ac685243b48eb237fa92fb6276 |
| 出典メモ | uspto-grants-2007_06 |