Potassium Carbonate → 5'-Chloro-2'-(2-methyl-2-propenyloxy)acetophenone

Temperatur

60 °C

A suspension of 5′-chloro-2′-hydroxyacetophenone (0.86 g, 5.0 mmol), potassium carbonate (1.4 g, 10 mmol) and 3-bromo-2-methylpropene (0.56 mL, 5.5 mmol) in anhydrous N,N-dimethylformamide (20 mL) was stirred at 60° C. for 4 hours. After cooling, the reaction mixture was diluted with water (100 mL), and the whole was extracted with ethyl acetate (100 mL). The organic layer was washed with saturated aqueous ammonium chloride solution (50 mL) and brine (50 mL) and dried over anhydrous magnesium sulfate. The solvent was removed in vacuo to give the title reference compound (1.1 g) as orange oil (Yield 96%).

1. temperatureAfter cooling
2. extractionthe whole was extracted with ethyl acetate (100 mL)
3. washThe organic layer was washed with saturated aqueous ammonium chloride solution (50 mL) and brine (50 mL)
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe solvent was removed in vacuo

ORD-Eintrag

ord-1609479122814f759c812f9af7a87ca2

Quelldatensatz

uspto-grants-2012_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08088817B2