反应详情

温度

50 °C

To a suspension of 2-((2-ethyl-2H-indazol-5-yl)methyl)isoindoline-1,3-dione (step-3 of Example 13, mixture) in MeOH (7 mL) was added hydrazine-H2O (0.5 mL), and the mixture was heated at 50° C. for 4 hrs. The mixture was concentrated, the residual white solid was added 2 M aqueous NaOH, and extracted with DCM, dried over Na2SO4, filtered and concentrated. The residual oil was diluted with MeOH and applied onto a strong cation exchange cartridge (BondElute (registered trademark) SCX, 1 g/6 mL, Varian Inc.), and the solid phase matrix was rinsed with MeOH (6 mL). The crude mixture was eluted with 1 M NH3 in MeOH (6 mL) and concentrated to give 68 mg (52% yield in 2 steps) of the titled compound as a colorless oil.

1. concentrationThe mixture was concentrated
2. additionthe residual white solid was added 2 M aqueous NaOH
3. extractionextracted with DCM
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. additionThe residual oil was diluted with MeOH
8. washthe solid phase matrix was rinsed with MeOH (6 mL)
9. washThe crude mixture was eluted with 1 M NH3 in MeOH (6 mL)
10. concentrationconcentrated