Zn^(2+)催化氟虫腈水解的产物及其结构表征

The Hydrolysis of Fipronil with Zn^(2+) Ion Catalysis and Its Crystal Structure

在溶剂热条件下,利用路易斯酸Zn2+对氟虫腈(5-氨基-1-(2,6-二氯-4-三氟甲基苯基)-4-三氟甲基亚磺酰基吡唑-3-腈)进行原位水解反应,得到其结晶产物5-氨基-1-(2,6-二氯-4-三氟甲基苯基)-4-三氟甲基亚磺酰基吡唑-3-羧酸.对该化合物进行了元素分析、红外、紫外-可见光谱测定及X-射线单晶衍射等表征.晶体结构解析表明该化合物属单斜晶系,空间群为P2(1)/n,晶胞参数为:a=12.7457(8),b=8.8244(6),c=15.7322(11),α=90°,β=100.2310(10)°,γ=90°,Z=4,V=1741.3(2)3,F(000)=856.化合物中存在的弱相互作用力分子间氢键将其形成一个稳定的三维层状结构.紫外-可见光谱分析表明该化合物在220 nm和281 nm处有最大吸收峰.

A new compound 1,5-amino-1-[2,6-dichloro-4-（trifluoromethyl） phenyl]-4-[（trifluoromethyl） sulfinyl]-1H-pyrazole-3-carboxylic acid has been produced by hydrothermal reaction of fipronil（5-amino-1-[2,6-dichloro-4-（trifluoromethyl） phenyl]-4-[（trifluoromethyl） sulfinyl]-1H-pyrazole-3-nitrile） and lewis acid ZnCl2.The compound was characterized by elemental analysis,IR spectra,and single-crystal X-ray diffraction.The crystal belongs to the monoclinic system,space group P21/c with a = 12.7457（8）,b = 8.8244（6）,c = 15.7322（11）,α= 90°,β = 100.2310（10）°,γ=90°,Z= 4,V = 1741.3（2） 3,F（000） = 856.The intermolecular hydrogen bonds are speculated to hold together the molecules of the compound.UV spectrum of 1 in solid state shows two maximum absorption peaks at 220 and 281 nm respectively.