化工社化工社化学信息打印报告 · 仅供科研参考
聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] → 5-(4-Iodo-pyridin-2-yloxy)-pyrimidine
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | 聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯] | HCID 962 | — |
| 反应物 | 氢化钠 | HCID 24758 | — |
| 反应物 | 5-羟基嘧啶 | HCID 565855 | — |
| 反应物 | 2-氟-4-碘吡啶 | HCID 7023570 | — |
| 溶剂 | N,N-二甲基甲酰胺 | HCID 6228 | — |
| 产物 | 5-(4-Iodo-pyridin-2-yloxy)-pyrimidine | HCID 66634994 | — |
反应步骤
To 259 mg (26.9 mmol) pyrimidin-5-ol (J. Chem. Soc. 1956, 2033) in 200 mL DMF are added 108 mg (26.9 mmol) sodium hydride (60% dispersion in mineral oil). The mixture is stirred for 20 min at r.t. After that time, 500 mg (22.4 mmol) 2-fluoro-4-iodopyridine are added and the mixture is stirred for 12 h at 80° C. Subsequently the mixture is poured into water and extracted with ethyl acetate (3×). The combined organic layers are washed with brine. After drying over sodium sulphate, the solvent is removed in vacuo and the residue is purified by column chromatography (silica gel; heptane/EtOAc, 100/0→40/60).
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US08530460B2 |
| 来源数据集 | uspto-grants-2013_09 |
| ORD ID | ord-758d3432bd7e4951ae9ed34d7b515c70 |
| 来源说明 | uspto-grants-2013_09 |