反应详情

A suspension of K2CO3 (235 mg, 1.70 mmol), 2-(bromomethyl)-1,3-dioxolane (400 mg, 1.70 mmol), and 3-methoxy-4-(2-(pyrrolidin-1-yl)ethoxy)benzenamine (3.0 g, 14.5 mmol), preparation described in Patent: WO2002/101146, in DMSO (17 mL) was heated at 80° C. for 24 hr. After removal of any precipitate by filtration, the filtrate was partitioned between EtOAc/H2O (100/20 mL). The organic layer was washed with brine and dried over MgSO4. After removal of the solvent under vacuum, the residue was chromatographed on silica gel using 0%-20% gradient EtOAc/Hexanes to elute the title compound as a yellow brownish oil (150 mg, 27%) MS (ESI) 323 (M+H)+.

1. customAfter removal of any precipitate
2. filtrationby filtration
3. customthe filtrate was partitioned between EtOAc/H2O (100/20 mL)
4. washThe organic layer was washed with brine
5. dry with materialdried over MgSO4
6. customAfter removal of the solvent under vacuum
7. customthe residue was chromatographed on silica gel using 0%-20% gradient EtOAc/Hexanes
8. washto elute the title compound as a yellow brownish oil (150 mg, 27%)