- Preparation method of stable isotope-labeled clorprenaline
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The invention relates to a preparation method of stable isotope-labeled clorprenaline. The preparation method comprises the following steps: with 2-bromo-2'-chloroacetophenone as an initial raw material, successively conducting improved Gabriel synthesis (wherein the initial raw material and an amination reagent sodium, namely diformyl amide are subjected to a nucleophilic substitution reaction), hydrolysis, reduction and reductive amination so as to synthesize the isotope-labeled clorprenaline . According to the preparation method disclosed by the invention, through a four-step conventional chemical reaction, process design is reasonable, raw material price is low, an experimental process is controllable, operation is simple and convenient, various required labeled compounds such as D-labeled, 13C-labeled or D/13C double-labeled compounds can be conveniently synthesized, the purity of the prepared target product is high and reaches 98% or above, total yield reaches 66% or above, the isotope abundance of the final product can reach 98% or above, the phenomenon of isotope abundance dilution is avoided, higher reproducibility and stability are achieved, and the obtained target compound can provide a standard reagent for accurately and quantitatively detecting trace residues of clorprenaline.
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- Method for preparing beta-arylamino alcohol drugs such as tulobuterol, clorprenaline, dichloroisoprenaline and sotalol
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The invention provides a method for preparing beta-arylamino alcohol drugs such as tulobuterol, clorprenaline, dichloroisoprenaline and sotalol. The beta-arylamino alcohol drugs have a chemical structure represented by a formula 4 shown in the description. The method comprises the following steps: (1) reacting arylethanone represented by a formula 1 shown in the description with a halogenating agent and sulfoxide to obtain arylglyoxal represented by a formula 2 shown in the description and or 1,1-dihydroxyarylethanone represented by a formula 3 shown in the description; and (2) performing a nucleophilic addition reaction on the arylglyoxal represented by the formula 2 and/or the 1,1-dihydroxyarylethanone represented by the formula 3 and an amine compound having a chemical formula of R1-NH2, and performing a reductive amination reaction in the presence of a reducing agent to obtain the beta-arylamino alcohol drugs.
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