反应详情

To 64 mg (0.08 mmol) of compound 120 was added 20 mL of saturated sodium carbonate, 76 mg of sodium hydrosulfite (Na2S2O4), and 2 mL of DMF. The reaction was allowed to stir at ambient temperature for 22 hours. Then, the reaction was extracted with ethyl acetate and 1 N HCl. The organic layer was dried (MgSO4), filtered, and the volatiles removed by rotary evaporation. The product was purified by reverse-phase HPLC (C18, 250×20 mm column) using trifluoroacetic acid (TFA) buffer system (Buffer A: 5% acetonitrile, 95% water, 0.05% TFA; Buffer B: 95% acetonitrile, 5% water, 0.05% TFA; 17 mL/min; 0–50% B in 10 min., 50% B for 17 min., 50–100% B in 20 min). Fractions containing the product were combined and lyophilized to provide 24 mg of compound 121.

1. extractionThen, the reaction was extracted with ethyl acetate and 1 N HCl
2. dry with materialThe organic layer was dried (MgSO4)
3. filtrationfiltered
4. customthe volatiles removed by rotary evaporation
5. customThe product was purified by reverse-phase HPLC (C18, 250×20 mm column)
6. wait0–50% B in 10 min.
7. wait50% B for 17 min.
8. wait50–100% B in 20 min)
9. additionFractions containing the product