反应详情

A solution of Example 6, F1 (2 eq), I2 (1 eq) and NaHCO3 (2.5 eq) in a mixture of CH3CN and H2O (20:1) was heated at reflux for 12 hrs and then the MeCN was removed under reduced pressure. The resulting residue was partitioned between DCM and water. The organic phase was washed with brine, dried (Na2SO4), filtered, concentrated under reduced pressure. The resulting brown oil was purified by Biotage system eluting with EtOAc/petroleum ether to obtain the desired compound. MS (ES) C33H38ClN5O6 requires: 635, found: 636 (M+H)+.

1. temperaturewas heated
2. temperatureat reflux for 12 hrs
3. customthe MeCN was removed under reduced pressure
4. customThe resulting residue was partitioned between DCM and water
5. washThe organic phase was washed with brine
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customThe resulting brown oil was purified by Biotage system
10. washeluting with EtOAc/petroleum ether