反应详情

A solution of N-cyclohexyl-N′-[3-({2-[(6-{[(2R)-2-(2,2-dimethyl-4H-1,3-benzodioxin-6yl)-2-hydroxyethyl]amino}hexyl)oxy]ethoxy}methyl)phenyl]urea (0.138 g) in acetic acid (4 ml) and water (1 ml) were stirred under nitrogen at 70° C. for 45 min. The reaction mixture was cooled to room temperature before concentrating under vacuum and azeotroping with MeOH (3×10 ml) to give a residue which was purified by Biotage. Elution with 50:8:1 dichloromethane:EtOH:ammonia followed by solvent evaporation in vacuo gave the title compound (0.126 g). LCMS RT=2.65 min, ES+ve 558 (MH)+.

1. concentrationbefore concentrating under vacuum
2. customazeotroping with MeOH (3×10 ml)
3. customto give a residue which
4. customwas purified by Biotage
5. washElution with 50:8:1 dichloromethane
6. customEtOH:ammonia followed by solvent evaporation in vacuo