反应详情

A solution of 5-(4-chlorobenzyl)-2,2-dimethyl-1,3-dioxane-4,6-dione (1.50 g, 5.58 mmol, Intermediate 3: step a) and 3 M aqueous NaOH (16 mL) was heated in the microwave at 75 W for 20 minutes at 120° C. The aqueous mixture was extracted with EtOAc (1×) then acidified to pH 1 with concentrated aqueous HCl and extracted with EtOAc (2×). The combined EtOAc extract was washed with H2O, brine and dried over Na2SO4, filtered. Solvents were removed under reduced pressure to afford the title compound as a white solid.

1. extractionThe aqueous mixture was extracted with EtOAc (1×)
2. extractionextracted with EtOAc (2×)
3. extractionThe combined EtOAc extract
4. washwas washed with H2O, brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. customSolvents were removed under reduced pressure