反应详情

To a CH2Cl2 (6 mL) solution of the title compound of Step A (1.40 g, 3.81 mmol) was added m-CPBA (77 wt %, 1.30 g, 5.70 mmol). After 15 h, 10 wt % Na2S2O5 (aq.) was added and the solution allowed to stir until the aqueous was KI paper negative and extracted with CH2Cl2 (2×). The combined organic layers were washed with saturated NaHCO3 (aq.), concentrated and treated with MeOH (30 mL) and 1N NaOH (15 mL). After 15 h, the reaction was partially concentrated to remove the MeOH and acidified with 1M KHSO4 then extracted with EtOAc (2×). The combined organic layers were dried and concentrated to give the 1.1 g of the title compound that was used in the next step without further purification.

1. extractionextracted with CH2Cl2 (2×)
2. washThe combined organic layers were washed with saturated NaHCO3 (aq.)
3. concentrationconcentrated
4. additiontreated with MeOH (30 mL) and 1N NaOH (15 mL)
5. waitAfter 15 h
6. concentrationthe reaction was partially concentrated
7. customto remove the MeOH
8. extractionthen extracted with EtOAc (2×)
9. customThe combined organic layers were dried
10. concentrationconcentrated