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Preparation technology of 2-aminopyridine-6-methyl formate

A technology of methyl formate and aminopyridine, which is applied in the field of preparation technology of 2-aminopyridine-6-methyl formate, can solve the problems of complex preparation technology and high cost, and achieve the effects of low cost and simple process

Inactive Publication Date: 2019-08-13
南京博源医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing manufacturing process of aminopyridine-methyl carboxylate compounds is complicated and costly, and there is an urgent need for a preparation process with simple production process and low cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1: Dissolve 2,4-dibromo-5-chlorotoluene in pyridine; add potassium permanganate aqueous solution dropwise to 2,4-dibromo-5-chlorotolylidine solution, stir to make 2, 4-dibromo-5-chlorotoluene is completely converted into 2,4-dibromo-5-chlorotoluene, filtered to obtain the manganese dioxide by-product, washed with distilled water for 8-10 times, and the manganese dioxide precipitate is dried at 110 degrees 4-5h to obtain manganese dioxide catalyst. Among them, the mass ratio of 2,4-dibromo-5-chlorotoluene and pyridine is 1:7; the mass ratio of potassium permanganate and distilled water is 1:3.5.

[0017] Mix 3-amino-4-methylpyridine with water, heat to 80°C, add manganese dioxide catalyst, add concentrated hydrochloric acid dropwise after stirring, stir and react for 2-3 hours, after cooling down to room temperature, add n-butanol after filtration, Heating to reflux for 3-4 hours, removing n-butanol by distillation under reduced pressure, performing multiple ext...

Embodiment 2

[0020] Embodiment two: the mass ratio of 2,4-dibromo-5-chlorotoluene and pyridine is 1:8, the mass ratio of potassium permanganate and distilled water is 1:3.5, in manganese dioxide catalyst and 3-amino-4 -The productive rate under the different mol ratios of picoline is shown in Table 2:

[0021] serial number Catalyst / Reactant Yield / % 1 0.065 / 6 89.52 2 0.075 / 3 93.77 3 0.095 / 6 90.52 4 0.112 / 4 92.57

[0022] Table 2

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Abstract

The invention discloses a preparation technology of 2-aminopyridine-6-methyl formate. By adopting the preparation technology, the problems are solved that production processes are complex and high incost. According to the technical scheme, 3-amino-4-methylpyridine serves as a raw material, after 3-amino-4-methylpyridine is mixed with water, manganese dioxide serving as a catalyst is added, afterstirring is conducted, concentrated hydrochloric acid is added dropwise, after reaction, the temperature of the mixture is reduced to room temperature, 1-butanol is added after filtration, and finally, dichloroethane is adopted to conduct extraction and then is removed through reduced pressure distillation to obtain 2-aminopyridine-6-methyl formate. The preparation technology of 2-aminopyridine-6-methyl formate is simple in process and low in cost and has great benefits to mass production.

Description

technical field [0001] The disclosure relates to the field of organic synthesis, in particular to a preparation process of 2-aminopyridine-6-carboxylic acid methyl ester. Background technique [0002] New compounds prepared by replacing benzene ring with pyridine have higher biological activity and lower toxicity, so pyridine intermediates have been developed rapidly. The existing preparation process of aminopyridine-methyl carboxylate compounds is complicated and costly, and a preparation process with simple production process and low cost is urgently needed. Contents of the invention [0003] The purpose of the present disclosure is to provide a preparation process of methyl 2-aminopyridine-6-carboxylate, so as to achieve the purpose of simple production and low cost. [0004] The above-mentioned technical purpose of the present disclosure is achieved through the following technical solutions: [0005] A preparation process for methyl 2-aminopyridine-6-carboxylate, com...

Claims

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Application Information

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IPC IPC(8): C07D213/79C07D213/803
CPCC07D213/79C07D213/803
Inventor 陈建国张国品
Owner 南京博源医药科技有限公司