916979-09-4Relevant articles and documents
Synthesis process of rifaximin-D6
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Paragraph 0031-0034, (2020/07/28)
The invention provides a synthesis process of rifaximine-D6, which comprises the following steps: 1) by using compounds I2-amino-4-methylpyridine and D2O as raw materials, reacting in the presence of5wt% palladium on carbon and under the protection of nitrogen to obtain a deuterated intermediate, i.e., a compound II 4-methyl-2-aminopyridine-D6; step 2), dissolving rifamycin S and the deuterated intermediate compound II 4-methyl-2-aminopyridine-D6 prepared in the step 1) into dichloromethane; under the protection of nitrogen, stirring at room temperature, dropwise adding a dichloromethane solution dissolved with elemental iodine, reacting at room temperature overnight for 18 hours, dropwise adding an L-ascorbic acid aqueous solution, stirring, and after the reaction is completed, washing and purifying to obtain the product rifaximin-D6. The synthesis method has the following technical effects that the synthesis method of the intermediate II of rifaximin-D6 is simple and convenient, andraw materials are easy to obtain; the steps for synthesizing rifaximin-D6 are simple and short, and the operation is easy.
General method of obtaining deuterium-labeled heterocyclic compounds using neutral D2O with heterogeneous Pd/C
Esaki, Hiroyoshi,Ito, Nobuhiro,Sakai, Shino,Maegawa, Tomohiro,Monguchi, Yasunari,Sajiki, Hironao
, p. 10954 - 10961 (2007/10/03)
A protocol of a versatile H-D exchange reaction of heterocyclic compounds catalyzed by heterogeneous Pd/C in D2O is described. The reaction of various nitrogen-containing heterocycles with 10% Pd/C (10 wt % of the substrate) under hydrogen atmosphere in D2O as a deuterium source at 110-180 °C for 24 h afforded the corresponding deuterated compounds with satisfactory efficiency of deuteration in moderate to excellent isolated yields. Furthermore, the Pd/C-H2-D2O system can be extended to the direct deuteration of biologically active compounds such as sulfamethazine, which is used as a synthetic antibacterial drug for fat stocks and would be applied as a general method for the preparation of the standard materials for the analysis of residual chemicals in foods and so on.