反应详情

Prepared by the same method as for 4-hydroxy-6-(2-phenylethyl)pyridazin-3(2H)-one (Example 1) from 3,4-bis(benzyloxy)-6-(1-phenylethenyl)pyridazine (Intermediate 25) except that upon completion of the reaction the resulting mixture was filtered through Celite washing with ethanol and then concentrated in vacuo to afford an orange solid. This was purified initially by eluting on a reverse phase C18 chromatography column (0-60% methanol in water with an acidic modifier) and upon combining and concentrating the appropriate fractions the crude product was recrystallised from a mixture of ethyl acetate and heptanes to afford a white solid and the final compound was recrystallised from a mixture of ethyl acetate and heptanes (32% yield).

1. filtrationwas filtered through Celite
2. washwashing with ethanol
3. concentrationconcentrated in vacuo
4. customto afford an orange solid
5. customThis was purified initially
6. washby eluting on a reverse phase C18 chromatography column (0-60% methanol in water with an acidic modifier) and
7. concentrationconcentrating the appropriate fractions the crude product
8. customwas recrystallised from a mixture of ethyl acetate and heptanes
9. customto afford a white solid