参与物
| 角色 | 名称 | HCID | 投料 |
|---|
| 反应物 | N-甲基哌嗪 | HCID 53167 | — |
| 反应物 | Methyl 4-((3-bromopyridin-2-yl)methoxy)benzoate | HCID 68725036 | — |
| 试剂 | 碳酸氢铯 | HCID 10796 | — |
| 催化剂 | 1,1'-联萘-2,2'-双二苯膦 (BINAP) | HCID 634876 | — |
| 催化剂 | 三(二亚苄基丙酮)二钯 | HCID 9811564 | — |
| 溶剂 | N,N-二甲基乙酰胺 | HCID 31374 | — |
| 产物 | Methyl 4-((3-(4-methylpiperazin-1-yl)pyridin-2-yl)methoxy)benzoate | HCID 68724671 | 64.22% |
反应步骤
A mixture of methyl 4-((3-bromopyridin-2-yl)methoxy)benzoate (360 mg, 1.12 mmol), Pd2dba3 (205 mg, 0.22 mmol), BINAP (278 mg, 0.45 mmol), cesium carbonate (728 mg, 2.23 mmol) and 1-methylpiperazine (168 mg, 1.68 mmol) in DMA (10 mL) was stirred at 100 °C for overnight. Sat. NaHCO3 aq was added to the mixture, extracted with ethyl acetate three times, the combined organics were dried over anhydrous Na2SO4, filtered, the filtrate was conc. in vacuo, the residue was purified with ISCO (50% ethyl acetate in hexant to 100% ethyl acetate to 40% mthanol in ethyl acetate) to yield a brown oil as methyl 4-((3-(4-methylpiperazin-1-yl)pyridin-2-yl)methoxy)benzoate (245 mg, 64.2 %).
来源与证据
| 来源数据集 | 750 AstraZeneca ELN dataset |
|---|
| ORD ID | ord-78ee6abad7ea4585a19ca47439cdac57 |
|---|
| 来源说明 | 750 AstraZeneca ELN dataset |
|---|
