反应详情

A solution of the title compound of step 1 (2.73 g, 10.95 mmol) in abs. dichloromethane (50 mL) was mixed with tert-BuOK (1.47 g, 13.14 mmol) and methyl iodide (747 μl, 12 mmol) at 0° C. in argon. After 30 min the batch was heated to RT and then stirred overnight (solid separated out). The reaction mixture was mixed with saturated NaCl solution (50 mL) and extracted with dichloromethane (3×30 mL). The combined organic phases were dried over Na2SO4, concentrated to low volume in a vacuum and the remaining residue was purified by flash chromatography with ethyl acetate/MeOH 20:1.

1. custom(solid separated out)
2. additionThe reaction mixture was mixed with saturated NaCl solution (50 mL)
3. extractionextracted with dichloromethane (3×30 mL)
4. dry with materialThe combined organic phases were dried over Na2SO4
5. concentrationconcentrated to low volume in a vacuum
6. customthe remaining residue was purified by flash chromatography with ethyl acetate/MeOH 20:1