D6-clorprenaline was synthesized with D6-acetone (99.9% atom D) and 2'-chloroacetophenone as starting materials. 2'-Chloroacetophenone is brominated by copper bromide to obtain 2-bromo-2'-chloroacetophenone. D6-isopropyl-amine was synthesized by reduction, bromination, amina-tion, hydrazinolysis and alkali hydrolysis reaction with D6-acetone. Then a one-pot method of amination and reduction was designed to synthesize D6-clorprenaline. The yield based on the amount of substance of D6-isopropyl-amine was 26.2%. The structure of target product was confirmed by NMR, MS, HPLC and X-ray crystal diffraction. Its chemical purity was higher than 98%, and isotopic abundance was 99.7% (atom D). The above compound could be used as an internal standard reagent for the determination of residual clorprenaline.