反应详情

温度

25 °C

A solution of the product from Example 1F (7.0 g, 37.0 mmol), EDAC (8.5 g, 44.3 mmol), HOBT (6.0 g, 44.4 mmol), and NMM (8.0 mL, 72.8 mmol) in DMF (30 mL) was stirred at 25° C. for 1 hour, treated with a solution of the product from Example 6A (14.15 g, 36.8 mmol) in DMF (30 mL), stirred at 25° C. for 16 hours, concentrated, and partitioned between ethyl acetate and saturated NaHCO3. The organic phase was washed with saturated NaHCO3 and brine, and concentrated. The solution of the residue in hot methanol (20 mL) and water (10 mL) was allowed to cool and stand for 16 hours. The solids were collected by filtration and rinsed several times with hexanes, followed by drying under vacuum to give the title compound (16.97 g, 77% yield).

1. concentrationconcentrated
2. custompartitioned between ethyl acetate and saturated NaHCO3
3. washThe organic phase was washed with saturated NaHCO3 and brine
4. concentrationconcentrated
5. temperatureto cool
6. waitstand for 16 hours
7. filtrationThe solids were collected by filtration
8. washrinsed several times with hexanes
9. customby drying under vacuum