反应详情

To a solution of compound 13-8 (40 mg, 0.073 mmol) in 3 mL of CH2Cl2 was added hexamethyldisilizane (0.3 mL), followed by bromo trimethylsilane (0.1 mL, 0.74 mmol). The reaction was allowed to stir for 18 h at ambient temperature. The organic solvent was removed in vacuo, followed by the addition of H2O (1 mL). The crude product was sonicated and yielded a white suspension. Solvent was removed in vacuo and the product was dissolved in DMSO (1.5 mL). The product was purified by prepatory HPLC using a 30-80% CH3CN with 0.05% trifluoroacetic acid gradient over 20 minutes. The pure fractions were combined and lyophilized to give the desired title compound 13-9. 1H NMR δ 7.35-7.41 (2H, m), 7.48-7.51 (3H, m), 7.56-7.66 (6H, m), 7.72-7.77 (4H, m); LC-MS: m/e 461(M+H)+.

1. customThe organic solvent was removed in vacuo
2. additionfollowed by the addition of H2O (1 mL)
3. customThe crude product was sonicated
4. customyielded a white suspension
5. customSolvent was removed in vacuo
6. dissolutionthe product was dissolved in DMSO (1.5 mL)
7. customThe product was purified by prepatory HPLC
8. waitgradient over 20 minutes