Cesium carbonate → Tetrafluoro-m-phenylenediamine dihydrochloride

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Reaction Steps

To a solution of 17-7 dihydrochloride (0.145 g, 0.3 mmole) in dried DMF (5 ml) is added Cs2CO3 (1.95 g, 0.6 mmole). The resulting mixture is stirred at r.t. for 5 min, 2-chloro-N,N-diethylacetamide (0.090 g, 0.6 mmole) is added dropwise and the mixture is stirred overnight. The reaction was then diluted with CH3CN (50 m), the inorganics filtered and the filtrate concentrated to a viscous residue. Flash chromatography over silica gel (CHCl3 -MeOH 92.5=7.5) provided pure free base, Rf =0.52 (CHCl3 /MeOH, 9:1). Treatment of the free base in EtOAc with HCl/Ether provided the dihydrochloride salt 17-8.

Provenance & Evidence