Reaktion #1080056

Reaktionsgleichung

3-(4-chloro-2-fluorophenyl)-1-methyl-6-trifluoromethyl-2(1H)-pyridone

chlorosulfonic acid

→

desired product

Ausbeute 86.0%

3-(4-chloro-5-chlorosulfonyl-2-fluorophenyl)-1-methyl-6-trifluoromethyl-2(1H)-pyridone

Ausbeute 86.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturby heating
2. 2
   TemperaturAfter cooling
3. 3
   Extraktionfollowed by extraction with ethyl acetate
4. 4
   WaschenAfter washing with water
5. 5
   Trocknena saturated sodium hydrogencarbonate aqueous solution, the organic layer was dried over anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONEthyl acetate was distilled off under reduced pressure
7. 7
   SonstigeThen, the obtained crude crystals
8. 8
   Waschenwere washed with n-hexane

Vorschrift

2.9 g (9.5 mmol) of 3-(4-chloro-2-fluorophenyl)-1-methyl-6-trifluoromethyl-2(1H)-pyridone was dissolved in 70 g of chlorosulfonic acid, followed by heating and stirring at 100° C. for 5 hours. After cooling, the mixture was gradually dropwise added to ice water, followed by extraction with ethyl acetate. After washing with water and a saturated sodium hydrogencarbonate aqueous solution, the organic layer was dried over anhydrous magnesium sulfate. Ethyl acetate was distilled off under reduced pressure. Then, the obtained crude crystals were washed with n-hexane to obtain 3.3 g (yield: 86%) of the desired product. Melting point: 77-78° C.

Quelle