反应详情

To an ice cold solution of the compound from Step 1 (525 mg, 1.6 mmol) in CH2Cl2 (16 mL) and MeOH (1.6 mL) was added MMPP (1.09 g, tech. 80%, 1.76 mmol). The resulting suspension was stirred at r.t. for 3 hrs. The reaction was diluted with EtOAc and a 1:1 mixture of H2O and saturated aqueous NaHCO3 and extracted. The aqueous layer was extracted one more time with EtOAc. The combined organic extracts were dried over MgSO4 and concentrated to dryness. The crude product was purified first by flash chromatography, eluted with EtOAc in hexane 35%, and then crystallized from EtOAc/Hexane (1:1, 20 mL) to give the title compound as a bright orange solid. m.p. 167-168° C.

1. extractionextracted
2. extractionThe aqueous layer was extracted one more time with EtOAc
3. dry with materialThe combined organic extracts were dried over MgSO4
4. concentrationconcentrated to dryness
5. customThe crude product was purified first by flash chromatography
6. washeluted with EtOAc in hexane 35%
7. customcrystallized from EtOAc/Hexane (1:1, 20 mL)