Synthesis And Crystal Structure Of O,O '-Di-N-Butyl-Alpha-(4-Trifluoro-Methylphenylamino)-2-Fluorophenyl Phosphonate Under Ultrasonic Irradiation

The Mannich-type addition of O,O-di-n-butyl phosphite to 2-fluorobenzaidehyde and p-trifluoromethylaniline was carried out without solvent in the presence of BF3 center dot Et2O under ultrasonic irradiation at 78 similar to 80 degrees C for 0.5 h to afford the title compound alpha-aminophosphonate 4 in good yield. The structure was verified by elemental analysis, H-1 NMR, IR and MS spectra. The X-ray diffraction analysis indicated that the crystal of compound 4 belongs to monoclinic system with space group P2(1)/c, a= 1.348(4) nm, b= 1.734(4) nm, c= 1.099(3) nm, alpha=90 degrees,beta= 109.71(4)degrees', gamma=90 degrees, V=2.417(11) nm(3), Z=4, D-c= 1.268 mu g/m(3), mu=0.166 mm(-1), F(000)=968. The final R=0.0727, wR(2)=0.1751 for 7780 unique reflections.