反应详情

A mixture of 14 g of the compound obtained in Step 4.4, 7.46 g of veratrylamine, 19.99 g of HBTU and 13.1 g of DIEA in 300 ml of DMF is stirred for 2 hours at room temperature. The solvent is evaporated off under reduced pressure and the residue is taken up in DCM. The resulting solution is washed twice with saturated aqueous NaHCO3 solution. The organic phase is dried over Na2SO4 and filtered, and the filtrate is evaporated under reduced pressure. The residue is chromatographed on silica gel, eluting with a PE/EtOAc mixture from (90/10, v/v) to (40/60, v/v) to give 16 g of the expected product.

1. customThe solvent is evaporated off under reduced pressure
2. washThe resulting solution is washed twice with saturated aqueous NaHCO3 solution
3. dry with materialThe organic phase is dried over Na2SO4
4. filtrationfiltered
5. customthe filtrate is evaporated under reduced pressure
6. customThe residue is chromatographed on silica gel
7. washeluting with a PE/EtOAc mixture from (90/10