Potassium Iodide → HCID 20227255, Verbindung

Chloroacetone (3.8 g, 3.3 ml, 41 mmol) was added dropwise to a solution of 3-bromo-4-fluoro-2-hydroxy-1-nitrobenzene (4.3 g, 18.2 mmol) in acetone (54 ml) with stirring at ambient temperature. Potassium carbonate (5.8 g, 42 mmol) and potassium iodide (6.0 g, 36.4 mmol), were added and the reaction mixture was heated to reflux temperature for 2 hours. The reaction mixture was then cooled to room temperature, poured onto water (100 ml), and extracted three times with ethyl acetate (150 ml). The combined organic layers were dried over magnesium sulfate, treated with decolorizing charcoal and filtered through diatomaceous earth. Solvent was removed in vacuo to afford a dark brown oil.

1. temperaturethe reaction mixture was heated
2. temperatureto reflux temperature for 2 hours
3. temperatureThe reaction mixture was then cooled to room temperature
4. additionpoured onto water (100 ml)
5. extractionextracted three times with ethyl acetate (150 ml)
6. dry with materialThe combined organic layers were dried over magnesium sulfate
7. additiontreated with decolorizing charcoal
8. filtrationfiltered through diatomaceous earth
9. customSolvent was removed in vacuo
10. customto afford a dark brown oil

ORD-Eintrag

ord-b5b5d443f0944165b5c2bde93a10cdc1

Quelldatensatz

uspto-grants-1986_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04623650