Reaktion #2330435

Reaktionsgleichung

4-Iodo-1-(3-methyl-4-nitrobenzyl)-3-trifluoromethyl-1H-pyrazole

heptafluoro-1-iodopropane

DMF

→

1-(3-methyl-4-nitrobenzyl)-4-pentafluoropropyl-3-trifluoromethyl-1H-pyrazole

Ausbeute 38.3%

Lösungsmittel

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated
2. 2
   TemperaturAfter cooling to room temperature
3. 3
   Filtrationan insoluble matter was filtered with Celite
4. 4
   Waschenwashed with ethyl acetate
5. 5
   EinengenThe filtrate was concentrated under the reduced pressure
6. 6
   Sonstigethe obtained residue was purified by silica gel column chromatography

Vorschrift

4-Iodo-1-(3-methyl-4-nitrobenzyl)-3-trifluoromethyl-1H-pyrazole (2.06 g), copper powder (0.95 g), heptafluoro-1-iodopropane (2.96 g) and DMF (14 ml) were set in an autoclave and heated and stirred for 8 hours, maintaining the inside temperature of 130-135° C. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate (50 ml) and an insoluble matter was filtered with Celite and washed with ethyl acetate. The filtrate was concentrated under the reduced pressure and the obtained residue was purified by silica gel column chromatography to obtain 1-(3-methyl-4-nitrobenzyl)-4-pentafluoropropyl-3-trifluoromethyl-1H-pyrazole (0.80 g).

Quelle