反应详情

(S)-dimethyl 2-((7-bromo-4-(chloromethyl)-1H-indazol-5-yl)methyl)succinate (630 mg, 1.6 mmol) was dissolved in acetonitrile (5 mL). Potassium carbonate (560 mg, 4.1 mmol) was added to the mixture followed by (aminomethyl)cyclopropane (700 μL, 8.1 mmol). Mixture was heated to reflux and held with stirring for 1.5 hours. Mixture was cooled to room temperature. Mixture was filtered. Filtrate was concentrated by roto-vap. Residue was dissolved in a mixture of toluene (10 mL) and acetic acid (1 mL). Mixture was heated to reflux and held with stirring for 18 hours. Mixture was concentrated by roto-vap. Silica gel chromatography (ethyl acetate-hexanes) afforded the title compound as tan solid in 64% yield. MS m/e (M+H)+=406.0, 408.0.

1. temperatureMixture was heated
2. temperatureto reflux
3. filtrationMixture was filtered
4. concentrationFiltrate was concentrated by roto-vap
5. dissolutionResidue was dissolved in a mixture of toluene (10 mL) and acetic acid (1 mL)
6. temperatureMixture was heated
7. temperatureto reflux
8. stirringwith stirring for 18 hours
9. concentrationMixture was concentrated by roto-vap