Study On Synthetic Processes Of Antitumour Active Organogermanium And Organphosphorus

In this paper, synthetic processes of two kinds of antitumour active organgermanium and one kind of organphosphorus were investigated. The two kinds of organgermanium were bis-β-carboxyethyl organogermanium sesquioxide (R-Ge-1) and bis-β-carbamylethyl organogermanium sesquioxide (R-Ge-2). The organphosphorus was adenosine 5'-monophosphate triethylamine (5'-AMPS).An improved synthetic process of β-carboxyethyl organogermanium sesquioxide (R-Ge-1) was studied. Germanium dioxide was used as the raw material, through deoxidization, addition, and hydrolysis, the product was gained. The optimum conditions to synthesizeβ-carboxyethyl organogermanium sesquioxide were established through orthogonal test: the time from beginning to adding sodium hypophosphite was 0.5h; the molar ratio of germanium dioxide, hydrochloric acid and sodium hypophosphite was 1:7.4:1.4; addition reaction time was 1.5h. And the yield was 69.7%. IR spectra and 1HNMR spectra were made to identify the product.An improved synthetic process of bis-β-carbamylethyl organogermanium sesquioxide (R-Ge-2) was studied. Germanium dioxide was used as the raw material, through deoxidization and addition, the intermediate was gained. The product was produced by reacting the intermediate with thionychloride and ammonia, and then hydrolyzing. The optimum conditions to synthesize bis-β-carbamylethyl organogermanium sesquioxide were established through orthogonal test. The temperature of acroyl haliding was 70℃,the temperature of aminating was 10℃; and the molar ration of ammonia and germanium dioxide was over 4.2. And the yield was 79.1%. IR spectra and 1HNMR spectra were also made to identify the product.An improved synthetic process of 5'-AMPS was studied.Adenosine was used as the raw material, dissolved in triethyl phosphate and then esterified with thiophosphoryl chloride under 0~5℃ for 8h without water and oxgen, in alkaline condition provided by 2,6-dimethylpyridine, introducing thiophosphoryl ester to adenosine.Then superfluous triethylamine was added and reacted under 5℃ for 1h to synthesize rough 5'-AMPS.The unpurified product was appled to a DEAE Sephadex A-25 column and eluted with triethylammonium bicarbonate. 13PNMR spectra was made to identify the product.