反应详情

温度

50 °C

A solution of 3-(3-{4-[(6-bromohexyl)oxy]but-1-ynyl}phenyl)imidazolidine-2,4-dione and 3-(3-{4-[(6-iodohexyl)oxy]but-1-ynyl}phenyl)imidazolidine-2,4-dione (3:1, 23.98 g) in acetonitrile (240 ml) and diisopropylethylamine (20 ml) was treated with (1R)-2-(benzylamino)-1-(2,2-dimethyl-4H-1,3-benzodioxin-6-yl)ethanol (18.22 g) and the mixture was heated to 50° C. for 5 days. The solvent was removed under reduced pressure, the residue was diluted with EtOAc (250 ml) and washed with water. The aqueous phase was re-extracted with EtOAc (75 ml) and the combined organic solutions were washed with brine, dried (MgSO4), and evaporated. The residue was purified by chromatography on flash silica gel eluting with dichloromethane-EtOAc (1:1) to give the title compound (17.25 g) LCMS RT=2.80 min

1. customThe solvent was removed under reduced pressure
2. additionthe residue was diluted with EtOAc (250 ml)
3. washwashed with water
4. extractionThe aqueous phase was re-extracted with EtOAc (75 ml)
5. washthe combined organic solutions were washed with brine
6. dry with materialdried (MgSO4)
7. customevaporated
8. customThe residue was purified by chromatography on flash silica gel eluting with dichloromethane-EtOAc (1:1)