반응 #493764

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5-(2-chloro-4-fluorophenyl)-1,3-dimethyl-1H-pyrazol-4-amine

product

5-(2-chloro-4-fluorophenyl)-1,3-dimethyl-1H-pyrazol-4-amine

4-chloro-2-fluoroiodobenzene

sodium tert-butoxide

→

title compound

4-(4-chloro-2-fluorophenyl)-5-(2-chloro-4-fluorophenyl)-1,3-dimethyl-1H-pyrazol-4-amine

용매

toluene

반응 조건

후처리

1. 1
   기타The resulting material was purified by flash chromatography on a silica gel (40 g), Varian Bond
2. 2
   세척Elute SI® column (30% ethyl acetate in hexanes as eluant)

실험 절차

A mixture of 5-(2-chloro-4-fluorophenyl)-1,3-dimethyl-1H-pyrazol-4-amine (i.e. the product of Step F) (7.07 g, 23.8 mmol), 4-chloro-2-fluoroiodobenzene (256 μL, 2.0 mmol), sodium tert-butoxide (0.192 g, 2.0 mmol) and [1,1′-bis(diphenylphosphino)ferrocene]-dichloropalladium(II) (0.117 g, 0.16 mmol) in toluene (5 mL) was heated at 180° C. in a Biotage Initiator™ microwave apparatus for 1 h. The resulting material was purified by flash chromatography on a silica gel (40 g), Varian Bond Elute SI® column (30% ethyl acetate in hexanes as eluant) to provide the title compound, a compound of the present invention, as a dark purple/brown oil (164 mg).

출처