Reaktion #348151

Reaktionsgleichung

2-chloro-5-[4-chloro-1-methyl-5-(trifluoromethyl)-1H-pyrazol-3-yl]-4-fluorobenzenemethanol

K2CO3

isopropyl bromoacetate

→

((2-chloro-5-(4-chloro-1-methyl-5-(trifluoromethyl)-1H-pyrazol-3-yl)-4-fluorophenyl)methoxy)acetic acid, 1-methylethyl ester

Ausbeute 41.0%

Lösungsmittel

DMSO

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 purified chromatographically

Vorschrift

At 25° C., 1.7 g (5.0 mmole) 2-chloro-5-[4-chloro-1-methyl-5-(trifluoromethyl)-1H-pyrazol-3-yl]-4-fluorobenzenemethanol, 0.8 g (5.5 mmole) K2CO3 and 0.7 mL (5.5 mmole) isopropyl bromoacetate were slurried in 15 mL DMSO. The mixture was stirred overnight at 45° C. 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 purified chromatographically using 10% ethyl acetate in hexane as the eluent to give 0.9 g (41%) of ((2-chloro-5-(4-chloro-1-methyl-5-(trifluoromethyl)-1H-pyrazol-3-yl)-4-fluorophenyl)methoxy)acetic acid, 1-methylethyl ester as a white solid; mp 55° C.

Quelle