Reaktion #181

Reaktionsgleichung

Fc1ccc(Br)c(C(F)(F)F

CC(C)(C)OC(=O)N1CCNC

→

CC(C)(C)OC(=O)N1CCN(

Ausbeute 73.5%

Lösungsmittel

Cc1ccccc1

Reaktionsbedingungen

Vorschrift

In a 100ml sealtube was added 1-bromo-4-fluoro-2-(trifluoromethyl)benzene (0.91 g, 3.63 mmol), CESIUM CARBONATE (1.775 g, 5.45 mmol), CESIUM CARBONATE (1.775 g, 5.45 mmol), BINAP (0.271 g, 0.44 mmol), TERT-BUTYL 1-PIPERAZINECARBOXYLATE (0.812 g, 4.36 mmol), TRIS(DIBENZYLIDENEACETONE)DIPALLADIUM(0) (0.200 g, 0.22 mmol) and 18-CROWN-6 (0.115 g, 0.44 mmol). Followed by 15mL toluene. The mixture was degassed by N2 bubbling for 15min. The reaction mixture was heated at 110oC under nitrogen in an oil bath for overnight. The reaction mixture was diluted with ethyl acetate and filtered through celite. The Celite was washed with EtOAC. The EtOAC was concentrated down to give a brown oil. The crude product was purified by silica gel column(40g) and was eluted with 0% EtOAC/Hexane -25% EtOAC/Hexane. Yield: 0.93g Yellow oil. .

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