A novel and mild synthesis method of deuterated carbamate compounds (3a'~3c') was designed. Organic phenol as raw material, the intermediate chloroformate(2a~2c) was prepared by triphosgene under the NaOH as the catalyst, the target compound carbamate compounds (3a'~3c') was obtained by condensation with methylamine-D3-hydrochloride. Synthesis route can avoid the use of highly toxic isocyanate, and had the advantages of simple operation, short process flow, less side product, the yield of carbamate compounds was more than 60%, deuterium labeled isotope abundance is not diluted. The product was characterized by HPLC、MS、 1H NMR and 13C NMR, the chemical purity was more than 99%, the deuterium enrichment was more than 99 atom% .