Reaktion #666431

Reaktionsgleichung

sodium methanesulfinate

4-fluorophenacyl chloride

ethanol

→

1-(4-fluorophenyl)-2-methylsulfonylethan-1-one

Ausbeute 86.1%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated
2. 2
   Temperaturto reflux for 1 hour
3. 3
   FiltrationThe precipitated solids were collected by filtration
4. 4
   Waschenwashed with water
5. 5
   Sonstigedried
6. 6
   workup.DISSOLUTIONThe solids were dissolved in ethyl acetate
7. 7
   Trocknendried over anhydrous sodium sulfate
8. 8
   Einengenconcentrated under reduced pressure
9. 9
   SonstigeThe resulting residue was purified by recrystallization (hexane—ethyl acetate) acetate)

Vorschrift

To a 1 L volume four-necked flask, sodium methanesulfinate (31.3 g), 4-fluorophenacyl chloride (21-b) (48.1 g), and ethanol (300 ml) were added under a nitrogen atmosphere, and heated to reflux for 1 hour. After the mixture was cooled to room temperature, water (500 ml) was added. The precipitated solids were collected by filtration, washed with water, and dried. The solids were dissolved in ethyl acetate, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The resulting residue was purified by recrystallization (hexane—ethyl acetate) acetate) to give 51.9 g of 1-(4-fluorophenyl)-2-methylsulfonylethan-1-one (7-2-3).

Quelle