3 results about "O-nitrobenzaldehyde" patented technology

The present application relates to the technical field of nitrofurans metabolite content determination, and particularly relates to a method for determining the residual amount of nitrofurans metabolite in propolis. The method is that the pretreated propolis sample is detected by liquid chromatography-tandem mass spectrometry after gradient elution of the mobile phase; the pretreatment is that the propolis sample is sequentially hydrolyzed by hydrochloric acid, purified by HLB solid phase extraction column, derivatized by o-nitrobenzaldehyde, and purified by ethyl acetate treatment. The present application purifies the propolis sample after hydrochloric acid hydrolysis before o-nitrobenzaldehyde derivatization, so that o-nitrobenzaldehyde fully reacts with the nitrofurans metabolite in propolis, and the residual amount of nitrofurans metabolite in propolis is accurately detected by combining the selection and gradient elution of the mobile phase.

The application discloses o-nitrobenzaldehyde and a synthesis method thereof, and belongs to the technical field of medical intermediates. The synthesis method comprises the following steps: dissolving o-nitrotoluene, dibromohydantoin and azobisisobutyronitrile in mixed organic solvents to perform a bromination reaction, then performing filtration, impurity removal, extraction and organic phase drying in sequence, and separating o-nitrodibromobenzene; adding the o-nitrodibromobenzene into a DMSO solution, adding calcium carbonate to perform an oxidation reaction, then performing filtration, extraction, organic phase drying and purification and decoloration in sequence, and obtaining o-nitrobenzaldehyde. The o-nitrobenzaldehyde is obtained through a bromination oxidation two-step reaction, the synthesis method has the advantages of simple process, low cost, small pollution and high product yield.

This invention discloses a method for preparing 3,5-dibromo-o-aminobenzaldehyde, belonging to the field of pharmaceutical intermediate synthesis technology. The method includes a reduction step, a bromination step, and a purification step. In the reduction step, o-nitrobenzaldehyde is used as raw material, and is obtained by iron powder reduction, toluene extraction, and dilute sulfuric acid back-extraction to obtain an aqueous solution of o-aminobenzaldehyde sulfate. In the bromination step, a hydrogen peroxide and hydrobromic acid system is used for the bromination reaction to obtain a crude product and a centrifuged acid mother liquor. The centrifuged acid mother liquor is decolorized, concentrated, and the dilute sulfuric acid is recovered and reused in the reduction step. In the purification step, the crude product is dissolved in acetone, crystallized, and dried to obtain a refined product. The acetone mother liquor is decolorized and subjected to multi-stage distillation to recover acetone for recycling. This invention achieves the recycling of dilute sulfuric acid and acetone, significantly reducing waste emissions, lowering production costs, and improving product yield and purity. It has the advantages of being green, environmentally friendly, economical, and efficient, and is suitable for industrial production.