1173021-09-4Relevant academic research and scientific papers
Preparation method of stable isotope labeled clenproperol
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, (2021/07/09)
The invention relates to a preparation method of stable isotope labeled clenproperol, which comprises the following steps: by taking 4-amino-3,5-dichloroacetophenone (II) as a raw material, carrying out bromination reaction to prepare a compound (III), then carrying out improved Gabriel synthesis reaction, namely amination reaction with sodium diformamide to obtain a compound (IV), then carrying out hydrolysis and reduction to obtain a compound (VI), and carrying out reductive amination reaction to generate a target compound (I). The preparation method disclosed by the invention is reasonable in process design, low in raw material price, controllable in experimental process and simple and convenient to operate, various required labeled compounds such as D-labeled, 13C-labeled or D/13C double-labeled compounds can be conveniently synthesized, and the prepared target product is high in purity, can be used as an internal standard substance in the field of food safety detection, and has important practical application value.
Stable isotope labeling Clenproperol compound and synthesis method thereof
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Paragraph 0184-0185, (2018/02/04)
The invention relates to a stable isotope labeling Clenproperol compound and a synthesis method thereof. The method comprises the following steps of (1) using stable isotope labeling 2,6-dichloroaniline as raw materials to generate stable isotope labeling 3,5-dichloro-4-aminoacetophenone through Friedel-Crafts acyl reaction; (2) performing bromination on the stable isotope labeling 3,5-dichloro-4-aminoacetophenone to obtain stable isotope labeling 3,5-dichloro-4-amino-alpha-bromo acetophenone; (3) enabling the stable isotope labeling 3,5-dichloro-4-amino-alpha-bromo acetophenone and isopropylamine to take a reaction for obtaining stable isotope labeling 1-(4-amino-3,5-dichlone)-2-isopropyl amino ethyl ketone; (4) enabling the stable isotope labeling 1-(4-amino-3,5-dichlone)-2-isopropyl amino ethyl ketone and a reducing agent to take a reaction to generate stable isotope labeling Clenproperol. The stable isotope labeling Clenproperol compound and the synthesis method have the advantages that the process route is simple; the synthesis is easy; the stable isotope atom utilization rate is high; the obtained product can be easily separated and purified; the chemical purity and the fractional isotopic abudance are 99 percent or higher; the trace detection requirements in the food safety field can be sufficiently met.
