Reaktion #1473116

Reaktionsgleichung

water

3-(4-chloro-2-fluoro-5-nitrophenyl)-1-methyl-6-trifluoromethyl-2(1H)-pyridone

tin

hydrochloric acid

→

desired product

Ausbeute 100.2%

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

Ausbeute 100.2%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAfter completion of the reaction
2. 2
   FiltrationInsoluble substances were filtered off
3. 3
   Extraktionthe filtrate was extracted 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 diisopropyl ether

Vorschrift

1.0 g (2.8 mmol) of 3-(4-chloro-2-fluoro-5-nitrophenyl)-1-methyl-6-trifluoromethyl-2(1H)-pyridone and 1.3 g (11 mmol) of tin were suspended in 30 ml of ethanol, and 5 ml of concentrated hydrochloric acid was added at room temperature, followed by stirring for 1 hour. After completion of the reaction, the reaction solution was poured into water and neutralized. Insoluble substances were filtered off, and the filtrate was extracted 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 diisopropyl ether to obtain 0.90 g (yield: 98%) of the desired product. Melting point: 155-157° C.

Quelle