反应详情

温度

90 °C

A mixture of 18b (1.1 g, 5.9 mmol), 6a (1.5 g, 4.84 mmol) and diisopropylethylamine (3 mL, 18.1 mmol) in 15 mL of DMF was heated at 80° C. for 17 h and at 90° C. for 24 h. The mixture was diluted with 100 mL of DCM, washed with brine (3×50 mL) and the extracts were dried, filtered and concentrated under vacuum. The residue was purified by flash chromatography (elution with 50-100% ethyl acetate and 0.1% TEA in hexanes) and finally purified on preparative HPLC to afford 0.3 g (14%) of 18-1. tR=5.21 (Method 5). EC50: 611 nM.

1. washwashed with brine (3×50 mL)
2. customthe extracts were dried
3. filtrationfiltered
4. concentrationconcentrated under vacuum
5. customThe residue was purified by flash chromatography (elution with 50-100% ethyl acetate and 0.1% TEA in hexanes)
6. customfinally purified on preparative HPLC