反应详情

温度

130 °C

3-Amino-N-methoxy-N-methyl-5-(pentafluorosulfanyl)benzamide (O5.075; 6.3 g) was dissolved in DMF (80 ml), and cesium carbonate (10.1 g), sodium iodide (0.62 g) and bis(2-bromoethyl) ether (19.37 g) were added. The mixture was divided between 10 microwave vessels, each of which was heated to 130° C. for 3 h. Subsequently, the batches were combined and freed of solvent. The residue was taken up in EA and washed with water. The EA phase was dried and concentrated. The residue was purified using silica gel (120 g cartridge, n-heptane/EA gradient of 0-100% within 30 min). 2.48 g of the title compound were obtained. LC-MS rt: 1.41 min [M+H]+: 377.0 (met. a)

1. washwashed with water
2. dry with materialThe EA phase was dried
3. concentrationconcentrated
4. customThe residue was purified
5. customsilica gel (120 g cartridge, n-heptane/EA gradient of 0-100% within 30 min)