【摘 要】
:
采用BF3?Et2O催化和45kHz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,0.5h即可以较高收率获得目标化合物α-氨基膦酸酯(4),
【机 构】
:
贵州大学精细化工研究开发中心教育部绿色农药与农业生物工程重点实验室,贵州大学精细化工研究开发中心教育部绿色农药与农业生物工程重点实验室,贵州大学精细化工研究开发中心教育部绿色农药与农业生物工程重点实验
论文部分内容阅读
采用BF3?Et2O催化和45kHz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,0.5h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,1HNMR,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,Dc=1.268μg/m3,μ=0.166mm-1,F(000)=968.
Using BF3-Et2O as catalyst and butyl phosphite and o-fluorobenzaldehyde under 45 kHz ultrasonic irradiation, the Mannich reaction of trifluoromethylaniline was carried out at 78-80 ℃ with no solvent, The target compound α-amino phosphonate (4) was confirmed by elemental analysis, 1HNMR, IR and MS. The X-ray diffraction of the crystal structure of the compound showed that the compound belongs to the monoclinic space group P2 (1) / c = 1.099 (3) nm, α = 90 °, β = 109.71 (4) °, γ = 90 °, V = 2.417 (11) nm3, Z = 4, Dc = 1.268 μg / m3, μ = 0.166 mm-1, F (000) = 968.
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