Potassium Iodide → 1-(2-Hydroxy-4-((4-methoxyphenyl)methoxy)phenyl)ethanone

2′,4′-Dihydroxyacetophenone (11.71 g, 0.077 mol), 4-methoxybenzyl chloride (10.44 ml, 0.077 mol), anhydrous potassium carbonate (11.75 g, 0.085 mol) and potassium iodide (12.78 g, 0.077 mol) are heated together in refluxing dry acetone (80 ml) for 4 hours. The mixture is then cooled to room temperature, poured into water (250 ml) and extracted with ethyl acetate (3×100 ml). The ethyl acetate extracts are combined, washed with saturated brine (100 ml), dried (MgSO4), filtered and concentrated, until crystallization commences. After standing at 4° C. for 16 h, the crystals are recovered by filtration, washed with cold ethyl acetate and then with n-hexane and dried.

1. extractionextracted with ethyl acetate (3×100 ml)
2. washwashed with saturated brine (100 ml)
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated, until crystallization commences
6. filtrationthe crystals are recovered by filtration
7. washwashed with cold ethyl acetate
8. dry with materialwith n-hexane and dried

ORD-Eintrag

ord-7b4b11184e3f449b88142c800caa6db1

Quelldatensatz

uspto-grants-2010_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07732435B2