反应详情

温度

65 °C

To a solution of caesium carbonate (1.63 g, 5.0 mmol) in DMF (10 ml) was added 2-tert-butoxycarbonylamino-3-fluoro-benzoic acid from Example 19A (1.15 g, 4.5 mmol), (2-bromoethoxy)-tert-butyldimethylsilane (1.08 g, 4.5 ml) and sodium iodide (680 mg, 4.5 ml). The mixture was heated at 65° C. for 3 h and evaporated in vacuo. The residue was partitioned between chloroform and brine and the organic phase was dried and evaporated in vacuo. The residue was purified by flash chromatography on silica (eluant EtOAc: pet. ether 15:85) to give a colourless gum; yield 1.1 g, 59%.

1. customevaporated in vacuo
2. customThe residue was partitioned between chloroform and brine
3. customthe organic phase was dried
4. customevaporated in vacuo
5. customThe residue was purified by flash chromatography on silica (eluant EtOAc: pet. ether 15:85)
6. customto give a colourless gum