反应详情

A microwave vial was charged with 5-{(1R)-2-[(3R)-3-aminopyrrolidin-1-yl]-1-hydroxyethyl}-4-methyl-2-benzofuran-1(3H)-one hydrochloride [INTERMEDIATE 4] (100 mg, 0.32 mmol), 4-methyl-5-[(2R)-oxiran-2-yl]-2-benzofuran-1(3H)-one [INTERMEDIATE 2B] (61 mg, 0.32 mmol), MP-carbonate resin (200 mg), and ethanol (1 mL). The reaction mixture was heated in a microwave reactor at 150 C for 1 hour, and then cooled, filtered and concentrated in vacuo. The resulting residue was dissolved in DMSO (1 mL) and purified by HPLC to provide 5-{(1R)-1-hydroxy-2-[(3R)-3-{[(2R)-2-hydroxy-2-(4-methyl-1-oxo-1,3-dihydro-2-benzofuran-5-yl)ethyl]amino}pyrrolidin-1-yl]ethyl}-4-methyl-2-benzofuran-1(3H)-one.

1. temperatureThe reaction mixture was heated in a microwave reactor at 150 C for 1 hour
2. temperaturecooled
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. dissolutionThe resulting residue was dissolved in DMSO (1 mL)
6. custompurified by HPLC