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The preparation method of 2-aminopyrimidine

An aminopyrimidine and temperature control technology, which is applied in the fields of medicine and chemical industry, can solve problems such as low yield, loss of life and property, and difficult control, and achieve the effect of simple synthesis operation, good reaction selectivity, and mild reaction conditions

Active Publication Date: 2014-10-22
NEW FOUNDER HLDG DEV LLC +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] Above-mentioned method all can make 2-aminopyrimidine, and method 1, 2 all will use zinc powder reduction dechlorination, and this operation is not easy to control and raw material is not easy to obtain, and production cost is high; Method 3 will use highly corrosive chlorosulfonic acid and For some heavy metal catalysts, the simultaneous operation is not easy to control, the yield is low, and the production cost is high; method 4 catalyst strong acid ion exchange resin is not easy to get, and the production cost is high, so it is not suitable for industrial production; method 5 will use highly toxic chemical phosgene, This chemical is not only difficult to produce and store, but once it leaks, it will cause immeasurable loss of human life and property, and cause relatively large environmental pollution accidents and social impact. At the same time, the use of highly toxic solvent benzene will cause harm to operators and the environment. greater damage

Method used

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  • The preparation method of 2-aminopyrimidine
  • The preparation method of 2-aminopyrimidine
  • The preparation method of 2-aminopyrimidine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1) Preparation of added aldehyde oil (compound IV):

[0032] Add 145g of kerosene into the reaction vessel, and put in 19.5g of industrial N,N-dimethylformamide (DMF), and control the temperature of the material during the feeding process to not exceed 50.0°C. Control the temperature at 30.0-50.0°C and add industrial N,N-dimethylformamide (DMF) dropwise, then control the temperature at 30.0-40.0°C and add 20.6g of industrial phosphorus trichloride dropwise, and then control the temperature at 30.0-40.0 36 g of acetaldehyde diethyl acetal was added dropwise. After the dropwise addition, continue to stir for 20-30 minutes. When the temperature of the material does not rise any more (generally it will rise to 35.0-45.0°C), raise the temperature of the system to 45.0-55.0°C and let it stand for 15-20 minutes. Kerosene is used mechanically. Add 60g of industrial methanol to the lower layer solution and control the temperature at 0-20.0°C to obtain about 110g-120g of aldehyd...

Embodiment 2

[0036] 1) Preparation of added aldehyde oil (compound IV):

[0037] Add 145kg of kerosene in the reaction tank, put into industrial N,N-dimethylformamide (DMF) 19.5kg, and control the temperature of the material during the putting into process to be no more than 50.0°C. Control the temperature at 30.0-50.0°C and continue to drop industrial N,N-dimethylformamide (DMF), then control the temperature at 30.0-40.0°C and add 21kg of industrial phosphorus trichloride dropwise; then control the temperature at 30.0-40.0 36 kg of acetaldehyde diethyl acetal was added dropwise. After the dropwise addition, continue to stir for 20-30 minutes. When the temperature of the material no longer rises (usually to 35.0-45.0°C), raise the temperature of the system to 45.0-55.0°C and let it stand for 15-20 minutes. For further application, add 60kg of industrial methanol to the lower layer solution and control the temperature at 0-20.0°C to obtain about 115kg of added aldehyde oil-methanol solutio...

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Abstract

The invention discloses a preparation method of 2-amino pyrimidine, which comprises the following steps: performing addition on low-cost industrial N,N-dimethylformamide used as an initial raw material, phosphorus trichloride and acetal to prepare addition aldehyde oil; and under the catalytic effect of sodium methoxide, performing pressurized reaction on the addition aldehyde oil and guanidine nitrate to prepare the 2-amino pyrimidine. Compared with the existing synthesis process, the method has the advantages of accessible and low-cost raw material, simple synthesis operation, mild reaction conditions, easiness in control, good reaction selectivity and high yield, and is suitable for industrial big production.

Description

technical field [0001] The invention relates to a synthesis method of an intermediate in the fields of medicine and chemical industry, in particular to a preparation process of 2-aminopyrimidine. Background technique [0002] 2-Aminopyrimidine (2-Aminopyrimidine, whose structural formula is shown in the following formula I) is an important pharmaceutical and chemical intermediate, and is also an important compound for the synthesis of many agricultural fungicides, sulfonamide herbicides or anxiolytics such as buspirone hydrochloride. intermediate. [0003] [0004] There are not many synthetic methods for 2-aminopyrimidines. The prior art is mainly obtained from various substituted aminopyrimidines such as 4,6-dichloropyrimidine and 4-chloropyrimidine through zinc powder reduction, etc., or from 2-substituted aminopyrimidines. The product is synthesized by pyrimidine such as 2-hydroxypyrimidine, and the product is synthesized by ring-closure reaction with tetraalkoxymalo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/42
Inventor 岑勇
Owner NEW FOUNDER HLDG DEV LLC