102074-19-1Relevant articles and documents
Efficient synthesis of 3-(bromomethyl)-5-methylpyridine hydrobromide
Guo, Jianyu,Lu, Yan,Wang, Jin
, p. 203 - 205 (2015)
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.
New impurity of rupatine fumarate and preparation method and detection method thereof
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Paragraph 0115, (2020/03/31)
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.
Preparation of 5-methyl-3-polybromide methylpyridinio hydrobromide method
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, (2019/02/02)
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.