反应详情

To a solution of compound 29c (275 mg, 0.420 mmol) in DCM (3 mL), TFA (2 mL) was added. The resulting mixture was stirred at rt for 2 h and concentrated. The residue obtained was dried under reduced pressure overnight and re-dissolved in EtOH (5 mL). Na2CO3 (1.00 g, 9.50 mmol) and 2-chloroquinoline (234 mg, 1.43 mmol) were then added and the resulting mixture was heated at reflux for 5 h. The reaction mixture was allowed to cool to rt, diluted with water (20 mL) and extracted with EtOAc (3×20 mL). The combined EtOAc extracts were dried over Na2SO4, filtered, and concentrated. The residue obtained was purified by flash column chromatography on silica gel (0:1-1:0 EtOA/heptane) to obtain compound 29d. Mass Spectrum (LCMS, ESI pos.) Calcd. for C39H39N9O3: 682.3 (M+H). Found 682.3.

1. concentrationconcentrated
2. customThe residue obtained
3. customwas dried under reduced pressure overnight
4. dissolutionre-dissolved in EtOH (5 mL)
5. temperaturethe resulting mixture was heated
6. temperatureat reflux for 5 h
7. temperatureto cool to rt
8. extractionextracted with EtOAc (3×20 mL)
9. dry with materialThe combined EtOAc extracts were dried over Na2SO4
10. filtrationfiltered
11. concentrationconcentrated
12. customThe residue obtained
13. customwas purified by flash column chromatography on silica gel (0:1-1:0 EtOA/heptane)