反应详情

A room temperature mixture of 13.8 g of product from Example 392 dissolved in 100 ml of acetic acid is treated, dropwise over 20 minutes, with 9.0 ml of 30% hydrogen peroxide. The reaction mixture is stirred at room temperature for 1 hour, concentrated in vacuo at 50° C., and extracted with ethyl acetate. The organic layer is washed 2× with saturated sodium bicarbonate, water and saturated sodium chloride, dried and concentrated in vacuo. The aqueous washes are combined and concentrated in vacuo to about 25 ml. The residue is saturated with solid potassium carbonate and extracted 2× with 200 ml of ethyl acetate. The organic phase is concentrated in vacuo to a solid which is triturated with hexane and collected to give 13.1 g of the desired product.

1. concentrationconcentrated in vacuo at 50° C.
2. extractionextracted with ethyl acetate
3. washThe organic layer is washed 2× with saturated sodium bicarbonate, water and saturated sodium chloride
4. customdried
5. concentrationconcentrated in vacuo
6. concentrationconcentrated in vacuo to about 25 ml
7. extractionextracted 2× with 200 ml of ethyl acetate
8. concentrationThe organic phase is concentrated in vacuo to a solid which
9. customis triturated with hexane
10. customcollected