Reaktion #348140

Reaktionsgleichung

4-(4-chloro-1-methyl-5-(trifluoromethyl)-1H-pyrazol-3-yl)-5-fluoro-2-nitrophenol

K2CO3

ethyl bromoacetate

→

(4-(4-chloro-1-methyl-5-(trifluoromethyl)-1H-pyrazol-3-yl)-5-fluoro-2-nitrophenoxy)acetic acid, ethyl ester

Ausbeute 99.0%

Lösungsmittel

acetone

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAt 25° C.
2. 2
   TemperaturThe mixture was cooled
3. 3
   Extraktionextracted four times with ethyl acetate
4. 4
   WaschenThe ethyl acetate extracts were washed with brine
5. 5
   Trocknendried over anhydrous MgSO4
6. 6
   SonstigeThe residue was recrystallized from methylcyclohexane

Vorschrift

At 25° C., 6.11 g (0.018 mole) 4-(4-chloro-1-methyl-5-(trifluoromethyl)-1H-pyrazol-3-yl)-5-fluoro-2-nitrophenol, 2.5 g (0.019 mole) K2CO3, and 2.0 mL (0.019 mole) ethyl bromoacetate were slurried in 100 mL acetone. The reaction mixture was stirred at 40° C. for 4 hours. The mixture was cooled, diluted with 100 mL cold water, and extracted four times with ethyl acetate. The ethyl acetate extracts were washed with brine, dried over anhydrous MgSO4, and stripped in vacuo. The residue was recrystallized from methylcyclohexane to give 7.5 g (99%) of (4-(4-chloro-1-methyl-5-(trifluoromethyl)-1H-pyrazol-3-yl)-5-fluoro-2-nitrophenoxy)acetic acid, ethyl ester as a light yellow solid, mp 95°-96° C.

Quelle