- New impurity of rupatine fumarate and preparation method and detection method thereof
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The invention provides a novel impurity (a compound shown in formula I) of lupatifen fumarate and a preparation method of the novel impurity. The novel impurity can be used for controlling the quality of the lupatifen fumarate and a preparation of the lupatifen fumarate, so that a foundation is set for effectively controlling the quality of lupatifen fumarate bulk drugs and a preparation of the lupatifen fumarate bulk drugs. (the formula structure is shown in the description), wherein an anion X are selected from F, Cl, Br and I; and preferably, the anion X is Br.
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- Preparation of 5-methyl-3-polybromide methylpyridinio hydrobromide method
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The invention relates to a method for preparing 5-methyl-3-bromomethylpyridine hydrobromide. The method comprises a step of preparing methyl 5-methyl nicotinate; a step of preparing 5-methyl-3-pyridinemethanol; a step of preparing 5-methyl-3-pyridinemethanol hydrobromide; and a step of preparing 5-methyl-3-bromomethylpyridine hydrobromide. In the step of preparing methyl 5-methyl nicotinate, esterification of 5-methyl nicotinic acid and thionyl chloride is carried out under heating reflux to obtain methyl 5-methyl nicotinate; in the step of preparing 5-methyl-3-pyridinemethanol, a reduction reaction of methyl 5-methyl nicotinate and sodium borohydride is carried out in an organic solvent to obtain 5-methyl-3-pyridinemethanol; in the step of preparing 5-methyl-3-pyridinemethanol hydrobromide, 5-methyl-3-pyridinemethanol reacts with hydrobromic acid to obtain 5-methyl-3-pyridinemethanol hydrobromide; and in the step of preparing 5-methyl-3-bromomethylpyridine hydrobromide, 5-methyl-3-pyridinemethanol hydrobromide reacts with hydrobromic acid in an organic solvent and water is removed from the reaction system to obtain 5-methyl-3-bromomethylpyridine hydrobromide. According to the method, 5-methyl-3-bromomethylpyridine hydrobromide is obtained by four steps; the process is simple; and yield is high.
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- Efficient synthesis of 3-(bromomethyl)-5-methylpyridine hydrobromide
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5-Methyl-3-(bromomethyl)pyridine is the key intermediate in the synthesis of rupatadine. In this article, a new preparation of 5-methyl-3-(bromomethyl)pyridine hydrobromide is reported, which used 5-methylnicotinic acid as the starting material, with a 65.9% overall yield. This method has the merits of being simple, efficient and environmentally friendly.
- Guo, Jianyu,Lu, Yan,Wang, Jin
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p. 203 - 205
(2015/08/24)
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- PYRAZOLOPYRIMIDINE DERIVATIVES AND USES AS ANTICANCER AGENTS
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Novel compounds having a fused pyrazolopyrimidine derivatives and related fused ring systems are disclosed. The compounds inhibit growth of a variety of types of cancer cells, and are thus useful for treating cancer. Pharmaceutical compositions, and methods of using these compounds and compositions to treat cancer and other diseases related to the dysregulation of kinase (such as Aurora A, Aurora B, Aurora C, cMet, JAK2, ROS1, but not limited to) pathways are disclosed. Efficacy of these compounds is demonstrated with a system for monitoring cell growth/migration, which shows they are potent inhibitors of growth and/or migration of cancer cells. Compositions comprising these compounds, and methods to use these compounds and compositions for treatment of cancers, are disclosed.
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