超声辐射下O,O'-二正丁基-α-(4-三氟甲基苯胺基)-2-氟苯基膦酸酯的合成与晶体结构

采用BF₃•Et₂O催化和45 kHz超声辐射下亚磷酸丁酯与邻氟苯甲醛、对三氟甲基苯胺在78～80 ℃, 无溶剂条件下进行类 Mannich 反应, 0.5 h即可以较高收率获得目标化合物α-氨基膦酸酯(4), 其结构经元素分析, ¹H NMR, IR及MS确认. 对化合物晶体结构进行X衍射分析, 结果表明化合物属单斜晶系, 空间群P2(1)/c, 晶胞参数a＝1.348(4) nm, b＝1.734(4) nm, c＝1.099(3) nm, α＝90°, β＝109.71(4)°, γ＝90°, V＝2.417(11) nm³, Z＝4, D_c＝1.268 g/m³, μ＝0.166 mm^－1, F(000)＝968.

Synthesis and Crystal Structure of O,O′-Di-n-butyl-α-(4-trifluoromethylphenylamino)-2-fluorophenylphosphonate under Ultrasonic Irradiation

The Mannich-type addition of O,O-di-n-butyl phosphite to 2-fluorobenzaldehyde and p-trifluoromethylaniline was carried out without solvent in the presence of BF₃•Et₂O under ultrasonic irradiation at 78～80 ℃ for 0.5 h to afford the title compound -aminophosphonate 4 in good yield. The structure was verified by ele-mental analysis, ¹H 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, α＝90°, β＝109.71(4)°, γ＝90°, V＝2.417(11) nm³, Z＝4, D_c＝1.268 g/m³, ＝0.166 mm^－1, F(000)＝968. The final R＝0.0727, wR₂＝0.1751 for 7780 unique reflections.