反应详情

A solution of N-(3-aminophenyl)-N′-[3-({2-({6-[(5R)-5-(2,2-dimethyl-4H-1,3-benzodioxin-6-yl)-2-oxo-1,3-oxazolidin-3-yl]hexyl}oxy)ethoxy}methyl)phenyl]-urea (0.20 g) in pyridine (4 ml) was treated under nitrogen at 20° with nicotinoyl chloride hydrochloride (0.118 g) and the mixture stirred for 5.5 h. Sat. sodium bicarbonate solution (25 ml) was added and the product was extracted with dichloromethane (3×20 ml). The combined organic layer was dried (Na2SO4) and the solvent removed in vacuo to give a residue that was purified by SPE. Elution with dichloromethane-EtOAc (1:0, 1:1, then 0:1), then MeOH-EtOAc (1:50), followed by solvent evaporation in vacuo gave the title compound (0.209 g). LCMS RT=3.54 min, ES+ve 738 (MH)+.

1. extractionthe product was extracted with dichloromethane (3×20 ml)
2. dry with materialThe combined organic layer was dried (Na2SO4)
3. customthe solvent removed in vacuo
4. customto give a residue that
5. customwas purified by SPE
6. washElution with dichloromethane-EtOAc (1:0, 1:1
7. custom0:1), then MeOH-EtOAc (1:50), followed by solvent evaporation in vacuo