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采用高效液相色谱-电喷雾质谱联用技术对芳硝基化合物选择性还原制羟胺的反应液进行直接分析,并对组分的结构进行了归属。对于不同溶剂中铁氧化物催化水合肼还原邻二硝基苯为邻硝基苯基羟胺的反应,分析表明,质子溶剂有利于邻二硝基苯还原,相同实验条件下,异丙醇为溶剂的反应体系中原料邻二硝基苯转化率高;乙醚为溶剂的反应体系中产物邻硝基苯基羟胺的选择性高。对于面包酵母还原芳硝基化合物制芳香羟胺的反应,芳环上具有吸电子取代基时,有利于得到芳香羟胺,在实验所选的一系列芳硝基化合物中,对1,2-二氰基-4-硝基苯还原的羟胺选择性大于98%。
High performance liquid chromatography-electrospray ionization mass spectrometry (HPLC-ESI-MS / MS) was used to directly analyze the reaction liquid of hydroxylamine by selective reduction of anthryl nitro compounds. The structure of the components was also assigned. For the different iron oxide catalytic hydrazine hydrazine hydrazine reduction o-nitrophenyl hydroxylamine reaction, analysis showed that the proton solvent is conducive to o-dinitrobenzene reduction under the same experimental conditions, isopropanol as a solvent The conversion of ortho-dinitrobenzene in the reaction system is high. The selectivity of o-nitrophenylhydroxylamine in the reaction system of diethyl ether is high. For baker’s yeast reduction of aryl nitro compounds to aromatic hydroxylamine reaction, the aromatic ring with electron-withdrawing substituents, is conducive to aromatic hydroxylamine, selected in a series of experimental nitro compounds, 1,2-dicyanide The base-4-nitrobenzene reduced hydroxylamine selectivity is greater than 98%.