反应详情

A mixture of compound 4a as obtained from the above Synthesis Ex. 1 (0.50 g, 2 mmol) and N-(2-hydroxyethyl)ethylenediamine (0.63 g, 6 mmol) in 2-ethoxyethanol (5 mL) was heated at 140-150° C. for 24 hrs (by TLC monitoring). After cooling, the reaction mixture was evaporated in vacuo to give a residue, which was dissolved in EA (50 mL). The EA layer was washed with H2O and brine and then dried (MgSO4). Concentration of the EA layer gave a residue, which was dissolved in MeOH (10 mL) and then added with a solution of 6N HCl at 0° C., followed by stirring at room temperature for 8 hrs. The resultant precipitate was filtered off, washed with MeOH, and dried at 90° C. under reduced pressure for 24 hrs to give the title compound 9 (0.50 g, 70% yield).

1. customas obtained from the above Synthesis Ex
2. temperatureAfter cooling
3. customthe reaction mixture was evaporated in vacuo
4. customto give a residue, which
5. washThe EA layer was washed with H2O and brine
6. dry with materialdried (MgSO4)
7. customConcentration of the EA layer gave a residue, which
8. filtrationThe resultant precipitate was filtered off
9. washwashed with MeOH
10. customdried at 90° C. under reduced pressure for 24 hrs