Preparation method for 4-amino-6-alkoxyl pyrimidine compounds

A technology for alkoxypyrimidine and amine compounds, which is applied in the field of preparation of 4-amino-6-alkoxypyrimidine compounds, can solve the problems of complicated operation, high content of impurity 3, low yield and the like, and achieves process simplification , High product yield, the effect of reducing energy consumption

Active Publication Date: 2012-06-27
浜田智子
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The higher the temperature in the ammonia or aminolysis reaction, the higher the content of impurities 1 and 2, which leads to a higher content of impurity 3 and a lower yield
The existing literature processes have the disadvantages of too long synthesis steps, cumbersome operation, uncontrollable reaction temperature in the ammonolysis reaction, high reaction pressure, high impurity content, and low yield, which need to be thoroughly improved

Method used

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  • Preparation method for 4-amino-6-alkoxyl pyrimidine compounds
  • Preparation method for 4-amino-6-alkoxyl pyrimidine compounds
  • Preparation method for 4-amino-6-alkoxyl pyrimidine compounds

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] In a 500ml four-necked bottle, it is equipped with a thermometer, a stirrer, a vent pipe, an exhaust gas absorption bottle, and water in the absorption bottle. Then add 250.0 g of water and 125.0 g of 4,6-dichloropyrimidine into the bottle, raise the internal temperature to 50-55°C in a hot water bath, replace the air in the kettle with ammonia gas twice, and feed ammonia gas under controlled flow rate, Stir the reaction, the exothermic reaction will cause the temperature of the system to rise, and the rate of passing ammonia should be such that the internal temperature of the reaction solution is 56-60°C, and there is basically no bubbles in the tail gas absorbing bottle. A total of 70g of ammonia is passed.

[0055] The reaction liquid was sampled for HPLC analysis, and the content of 4,6-dichloropyrimidine was 0.07156% (Area%), the content of 4-amino-6-chloropyrimidine was 98.5369% (Area%), and the content of impurity 2 was 0.6961% (Area%). Stop the reaction, lower t...

Embodiment 2～7

[0058] Change the ammonia total amount that feeds, other conditions are constant, repeat the operation in embodiment 1, gained result is as follows table:

[0059]

Embodiment 8～11

[0061] Ammonia total amount is fixed at 64.2g, changes the consumption of water, other conditions are constant, repeats the operation in embodiment 1, gained result is as follows:

[0062]

[0063]

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Abstract

The invention discloses a preparation method for 4-amino-6-alkoxyl pyrimidine compounds, wherein 4,6-dichloropyrimidine compounds wide, easy to get and low in price are used in the method. The method comprises the following steps of: obtaining 4,6-dichloropyrimidine compounds via atmospheric-pressure ammonolysis or aminolysis; mixing the 4,6-dichloropyrimidine compounds with alcohol compounds and an alkaline catalyst, and then perform reflux reaction; and treating the reaction solution to obtain the 4-amino-6-alkoxyl pyrimidine compounds. The preparation method disclosed by the invention has the advantages of being green and environment-friendly, simple and convenient in operation, low in cost, high in yield, low in the content of impurities and suitable for industrialized production.

Description

technical field [0001] The invention relates to a preparation method of 4-amino-6-alkoxypyrimidine compounds. According to the method of the invention, it is very convenient for large-scale production of 4-amino-6-methoxypyrimidine compounds. Background technique [0002] 4-amino-6-alkoxypyrimidine compounds, referred to as 4-MP, its structural formula is: [0003] R 1 , R 2 Represents a hydrogen atom, an alkyl group, R 1 , R 2 Can be the same or different; R 3 Represents an alkyl group; R 4 Represents hydrogen atom, alkyl group, amino group [0004] It is a synthetic raw material for many pesticides and medicines, especially sulfonamides, but there are few reports about its synthetic methods. [0005] Sulfonamides are still widely used all over the world because of their wide antibacterial spectrum, definite curative effect, stable properties, convenient storage and transportation, convenient oral administration, and low price; especially sulfa-6-methoxypyrimidine,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/47
Inventor 浜田申一浜田智子唐成见
Owner 浜田智子
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