Reaktion #158399

Reaktionsgleichung

1-(3,4,5-trifluoro-2-hydroxyphenyl)ethanone

morpholine

sulfur

hydrochloric acid

acetic acid

→

title compound

(3,4,5-trifluoro-2-hydroxyphenyl)acetic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturto cool to room temperature
2. 2
   workup.STIRRINGThe reaction mixture was stirred at 100° C. for 3 hr
3. 3
   Temperaturto cool to room temperature
4. 4
   Extraktionextracted with ethyl acetate
5. 5
   WaschenThe extract was washed with saturated brine
6. 6
   Trocknendried over anhydrous magnesium sulfate
7. 7
   Sonstigethe solvent was evaporated under reduced pressure
8. 8
   SonstigeThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

Vorschrift

A mixture of 1-(3,4,5-trifluoro-2-hydroxyphenyl)ethanone (7.5 g), p-toluenesulfonic acid monohydrate (0.375 g), morpholine (10 mL) and sulfur (2.0 g) was stirred at 120° C. for 5 hr, and allowed to cool to room temperature, and hydrochloric acid (20 mL) and acetic acid (20 mL) were added to the reaction mixture. The reaction mixture was stirred at 100° C. for 3 hr, allowed to cool to room temperature, and extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (6.0 g).

Quelle