residual product 0 06 g used directly in the next stage n m r cdcl 3 u03b4 2 55 2 82 bm 6h 2 94 3 24 bm 6h 3 63 bs 4h 6 40 7 06 complex 7h ppm 1 3 fluoro 4 aminophenyl 4 4 aminophenethyl piperazine 0 06 g was dissolved in pyridine 4 5 ml and methanesulphonyl chloride 0 13 g was added the mixture was stirred at room temperature overnight the pyridine removed by evaporation and the residue chromatographed over silica developing and eluting with 10 methanol in dichloromethane the fractions containing the product were evaporated to give a residue 0 30 g which was crystallized from methanol yielding the pure title compound 0 016 g m p 232 u00b0 4 u00b0 n m r cdcl 3 u03b4 2 54 m 6h 2 72 m 2h 2 89 s 3h 2 94 s 3h 3 14 m 4h 6 70 6 85 m 2h 7 08 7 12 3h 7 18 7 22 2h 9 35 vbs 2h ppm analysis found c 51 1 h 5 9 n 11 9 calculated for c 20 h 27 fn 4 o 4 s 2 c 51 0 h 5 8 n 11 9 1 acetylpiperazine 6 23 g 5 fluoro 2 nitrotoluene 7 51 g and sodium carbonate 5 12 g in dimethylformamide 40 ml were stirred at 100 u00b0 overnight evaporated and the residue partitioned between ethyl acetate and water the.