反应详情

The product from Example 15 (0.388 g, 0.84 mmol) was taken up in glacial acetic acid (25 mL), and zinc dust (2.8 g, 325 mesh) was added in portions over 3 minutes and was then stirred 2 hours at room temperature. The zinc was filtered off and washed with ethyl acetate and tetrahydrofuran. The organic solution was concentrated to dryness, the residue partitioned between ethyl acetate (200 mL) and sodium bicarbonate solution (200 mL), the organic layer washed with brine and dried (magnesium sulfate), filtered, concentrated, and the resulting solid triturated with hexanes/ethyl acetate, 3/1, v/v and the insoluble portion collected by filtration to give the product as a faintly yellow solid (0.296 g), mp 235-238° C.

1. filtrationThe zinc was filtered off
2. washwashed with ethyl acetate and tetrahydrofuran
3. concentrationThe organic solution was concentrated to dryness
4. customthe residue partitioned between ethyl acetate (200 mL) and sodium bicarbonate solution (200 mL)
5. washthe organic layer washed with brine
6. dry with materialdried (magnesium sulfate)
7. filtrationfiltered
8. concentrationconcentrated
9. customthe resulting solid triturated with hexanes/ethyl acetate, 3/1, v/v
10. filtrationthe insoluble portion collected by filtration