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 200 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