Determination method for 2-chloromethyl-3,5 dimethyl-4-methoxyl pyridine hydrochloride

Abstract

The invention provides a determination method for 2-chloromethyl-3,5dimethyl-4-methoxyl pyridine hydrochloride and belongs to an acidimetric non-aqueous titration method. The method comprises the following steps: by taking N-N-dimethylformamide as a titration solvent, a thymol blue absolute methanol solution as an indicator and lithium methoxide as a titrating solution, titrating until the blue color appears and calculating the content of 2-chloromethyl-3,5 dimethyl-4-methoxyl pyridine hydrochloride in a sample according to the consumed volume of the titrating solution, the concentration of the titrating solution and the sampling weighing amount of the sample. The method provided by the invention is one of the mainstream analytical methods. The method has the characteristics of being remarkable in finish point which is easy to judge, good in precision, high in accuracy and the like, can be used for accurately detecting the content of the 2-chloromethyl-3,5 dimethyl-4-methoxyl pyridine hydrochloride, and is simple, economic and rapid.

Description

technical field [0001] The invention relates to the detection of pharmaceutical raw materials, in particular to a method for determining 2-chloromethyl-3,5-dimethyl-4-methoxypyridine hydrochloride. Background technique [0002] 2-Chloromethyl-3,5-dimethyl-4-methoxypyridine hydrochloride (Omeprazole chloride) is an important intermediate for the synthesis of new gastric drug Omeprazole, Chinese name: Omeprazole chloride Compound, referred to as Omeprazole chloride, English name: Omeprazole chloride compound, English chemical name: 2-Chloromethyl-4-methoxy-3,5-dimethylpyridine hydrochloride, molecular formula is C 9 h 13 C l2 NO. At present, there is no unified national standard or industry standard for this substance, and most of them implement enterprise standards, and the content determination method is generally provided by the supplier. A specific method is: accurately weigh about 0.2g of the sample, dissolve it with 50ml of silver nitrate solution (0.1mol / L), add 2ml...

AI Technical Summary

Problems solved by technology

[0003] The above determination method is to titrate the chloride ion in Ogilvy chloride, and the chloride ion is only one of the substituents, which is not representative. It is an indirect method to convert the amount of Ogilvy chloride through the amount of chloride ion, which is not intuitive and has errors. Larger, not the mainstream determination and analysis method; secondly, the silver chloride precipitate produced by the reaction has strong adsorption, which leads to the discoloration of the end point and fades quickly, and the titration jump point is not obvious, so it is difficult to judge the reaction end point and accuracy not enough

Images