反应详情

A mixture of compound 6a (0.0417 g, 0.094 mmol) and TCDI (0.025 g, 0.14 mmol) in THF (2 mL) was stirred at room temperature for 45 min. The mixture was diluted with H2O (2 mL) and extracted with EtOAc (3×5 mL). The combined organic extracts were washed with H2O (15 mL), dried (MgSO4), and concentrated. The residue was dissolved in THF (2 mL). Boron trifluoride diethyl etherate was added to the solution, and the resulting mixture was stirred at room temperature for 1 h. The mixture was diluted with H2O (2 mL) and extracted with EtOAc (3×5mL). The organic layers were dried (MgSO4), and concentrated. The resultant compound 9a was used in the next reaction without further purification. MS m/z (MH+) 485.8.

1. extractionextracted with EtOAc (3×5 mL)
2. washThe combined organic extracts were washed with H2O (15 mL)
3. dry with materialdried (MgSO4)
4. concentrationconcentrated
5. dissolutionThe residue was dissolved in THF (2 mL)
6. additionBoron trifluoride diethyl etherate was added to the solution
7. stirringthe resulting mixture was stirred at room temperature for 1 h
8. additionThe mixture was diluted with H2O (2 mL)
9. extractionextracted with EtOAc (3×5mL)
10. dry with materialThe organic layers were dried (MgSO4)
11. concentrationconcentrated
12. customThe resultant compound 9a was used in the next reaction without further purification