反应详情

A solution of T3P (1.57M in THF, 0.42 ml) was added to a mixture of the product from example 34 step (viii) (0.15 g), N,N-dimethylethanolamine (0.08 ml), TEA (0.3 ml) and DMAP (0.02 g) in DMF (5 ml) and stirred at rt for 24 h. The mixture was partitioned between DCM/water, the organics separated, washed with aq NaHCO3 soln, brine, dried and evaporated under reduced pressure. The residue was purified by RPHPLC, then the product dissolved in MeCN (10 ml) and PS-TBD (0.1 g) added and left for 2 h. The mixture was filtered, the solvent evaporated under reduced pressure and the residue triturated with isohexane and filtered to afford the title compound, 0.034 g.

1. customThe mixture was partitioned between DCM/water
2. washthe organics separated, washed with aq NaHCO3 soln
3. dry with materialbrine, dried
4. customevaporated under reduced pressure
5. customThe residue was purified by RPHPLC
6. dissolutionthe product dissolved in MeCN (10 ml)
7. additionPS-TBD (0.1 g) added
8. waitleft for 2 h
9. filtrationThe mixture was filtered
10. customthe solvent evaporated under reduced pressure
11. customthe residue triturated with isohexane
12. filtrationfiltered