429658-95-7Relevant articles and documents
Main degradation products of dabigatran etexilate evaluated by LC-UV and LC-ESI-MS, degradation kinetics and in vitro cytotoxicity studies
Bernardi, Raquel M.,D'Avila, Felipe B.,Todeschini, Vítor,Andrade, Juliana M.M.,Fr?ehlich, Pedro E.,Bergold, Ana M.
, p. 660 - 666 (2015)
The present study reports the stability profile of an antithrombotic drug: dabigatran etexilate (DAB). The drug was subjected to thermal degradation at 60 °C and products formed were investigated by liquid chromatography-UV (LC-UV) and liquid chromatography-mass spectrometry (LC-ESI-MS). Chromatographic separation of the degradation products was performed on a GL Sciences Inc. Inertsil ODS-2 column (250 mm × 4.6 mm i.d., with a particle size of 5 μm and pore size of 110 ?) with mobile phase consisting of acetonitrile and ammonium acetate buffer (pH 5.5; 10 mmol L-1) (65:35, v/v) pumped at 1.0 mL min-1 flow rate. Column temperature was set at 30 °C and detection at 225 nm using a UV detector. LC-UV method previously validated was extended to LC-ESI-MS for the characterization of the degradation products (DP-01 and DP-02) formed, without complicated isolation or purification processes, based on retention times and confirmation of molecular weight. Degradation kinetics of DAB was also evaluated and could be described as a first-order process (R2 = 0.9900). Furthermore, no evidence of cytotoxicity in human mononuclear cells was observed for DAB degraded samples.
Preparation method of dabigatran etexilate intermediate
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Paragraph 0023; 0027-0029; 0033-0034, (2020/08/02)
The invention relates to a preparation method of a dabigatran etexilate intermediate. The preparation method comprises the following steps: (1) carrying out addition on a compound III as shown in thefollowing formula and hydroxylamine to obtain a compound II under the catalysis of an alkali reagent; and (2) putting the compound II obtained in the step (1) into an organic solvent, and carrying outhydrogenation reduction reaction under the action of a catalyst to obtain a compound I shown in the following formula, namely the target product ethyl 3-(2-(((4-formamidinophenyl) amino) methyl)-1-methyl-N-(pyridine-2-yl)-1H-benzimidazole-5-formamide) propionate. The compound III is used as an initial reactant, and the compound II is obtained through addition reaction so that the use of a large amount of hydrogen chloride gas for preparing the imine ester hydrochloride is avoided; the compound I is prepared by hydrogenating and reducing the compound II, the reaction conditions are mild, and the safety of the preparation process is improved; meanwhile, the preparation method is simple in process step, the product is easy to purify, large-scale synthesis can be realized, and the industrialdevelopment prospect is relatively high.
Benzimidazole medicinal acid composition for injection and preparation method and application thereof
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Paragraph 0061-0066, (2019/01/22)
The invention discloses a benzimidazole medicinal acid composition for injection and a preparation method and application thereof. The composition comprises benzimidazole medicinal acid as shown in the formula I, a cosolvent, injection water, optional exi