反应详情

To 670 mg of the product from step A (crude but assumed to be 0.8 mmol based on the previous reaction), cooled in an ice bath under argon, was added 3 mL of trifluroacetic acid. The resulting mixture was allowed to slowly return to room temperature and stir for 5 hours. The mixture was then partitioned between saturated NaHCO3 solution and ethyl acetate. The organic layer was separated, dried over MgSO4 and concentrated to 139 mg of a white solid (83% pure by LC). The aqueous layer was extracted twice with ethyl acetate and the combined organic layers were dried over MgSO4 and concentrated to 0.10 g of yellow oil (70% pure by LC). Obtain a total of 239 mg (0.37 mmol, 47% yield) of crude title product.

1. custombased on the previous reaction),
2. temperaturecooled in an ice bath under argon
3. customto slowly return to room temperature
4. customThe mixture was then partitioned between saturated NaHCO3 solution and ethyl acetate
5. customThe organic layer was separated
6. dry with materialdried over MgSO4
7. concentrationconcentrated to 139 mg of a white solid (83% pure by LC)
8. extractionThe aqueous layer was extracted twice with ethyl acetate
9. dry with materialthe combined organic layers were dried over MgSO4
10. concentrationconcentrated to 0.10 g of yellow oil (70% pure by LC)