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Synthesis method of 1,2-dimethyl-1,4,5,6-tetrahydropyrimidine

A technology of tetrahydropyrimidine and a synthetic method, applied in directions such as organic chemistry, to achieve the effects of high yield, simple reaction route and simple procedure

Inactive Publication Date: 2018-11-16
XIAN WONDER SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The method is simple in design, but still needs to use a metal catalyst, and the reaction temperature needs to reach 120°C, the reaction time is as long as 24h, and the yield is only 45%.

Method used

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  • Synthesis method of 1,2-dimethyl-1,4,5,6-tetrahydropyrimidine
  • Synthesis method of 1,2-dimethyl-1,4,5,6-tetrahydropyrimidine
  • Synthesis method of 1,2-dimethyl-1,4,5,6-tetrahydropyrimidine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1, the preparation of N-[3-(methylamino)propyl]-acetamide

[0030] In a 1000mL three-necked flask, add N-methylpropylenediamine (200g, 2.27mol), add dropwise acetyl chloride (182g, 2.31mol) under stirring, control the temperature within 20°C, after the dropwise addition, within 60°C Continue to react for 1h, stop the reaction, and set aside.

[0031] 2. Preparation of 1,2-dimethyl-1,4,5,6-tetrahydropyrimidine

[0032] Add 200mL of PPE to the N-[3-(methylamino)propyl]-acetamide solution obtained in the previous step, control the temperature at 80°C by microwave, and react for 2h. After completion, the product 1,2-di Methyl-1,4,5,6-tetrahydropyrimidine 240g, yield 94.42%.

Embodiment 2

[0034] 1, the preparation of N-[3-(methylamino)propyl]-acetamide

[0035] In a 1000mL three-necked flask, add N-methylpropylenediamine (200g, 2.27mol), add dropwise acetic anhydride (240g, 2.34mol) under stirring, control the temperature within 30°C, and continue the reaction for 1h after the dropwise addition is completed. Stop the reaction and set aside.

[0036] 2. Preparation of 1,2-dimethyl-1,4,5,6-tetrahydropyrimidine

[0037] Add 180mL of PPE to the N-[3-(methylamino)propyl]-acetamide solution obtained in the previous step, control the temperature by microwave at 70°C, and react for 1.5h. After completion, the product 1,2- Dimethyl-1,4,5,6-tetrahydropyrimidine 230g, yield 90.49%.

Embodiment 3

[0039] 1, the preparation of N-[3-(methylamino)propyl]-acetamide

[0040] In a 1000mL three-necked flask, add N-methylpropylenediamine (200g, 2.27mol), add acetic anhydride (2.49mol) dropwise under stirring, control the temperature within 25°C, after the dropwise addition is completed, continue the reaction for 1h and stop the reaction ,spare.

[0041] 2. Preparation of 1,2-dimethyl-1,4,5,6-tetrahydropyrimidine

[0042] Add 180mL of PPE to the N-[3-(methylamino)propyl]-acetamide solution obtained in the previous step, control the temperature at 60°C by microwave, and react for 1.8h. After completion, the product 1,2- Dimethyl-1,4,5,6-tetrahydropyrimidine 235g, yield 92.45%.

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Abstract

The invention discloses a synthesis method of 1,2-dimethyl-1,4,5,6-tetrahydropyrimidine. A novel route is chosen, reactions are efficiently and quickly carried out under the assistance of microwaves,and the product yield is high. The synthesis method has the advantages of simple reaction route, easy operation, short reaction time, and high yield.

Description

technical field [0001] The invention belongs to the field of fine chemical industry, and in particular relates to a synthesis method of compound 1,2-dimethyl-1,4,5,6-tetrahydropyrimidine. Background technique [0002] Compound 1,2-Dimethyl-1,4,5,6-tetrahydropyrimidine, the English name is: 1,2-Dimethyl-1,4,5,6-tetrahydropyrimidine. It is an important pharmaceutical intermediate, which can be used to prepare broad-spectrum, high-efficiency anthelmintic drug pyrantel; it can also be used to prepare lamivudine, which inhibits hepatitis B virus. It has important uses in the production of medicines. [0003] [0004] According to relevant information, the synthesis of 1,2-dimethyl-1,4,5,6-tetrahydropyrimidine is mainly CN101323595 published by Li Honggong et al. The synthesis route is: [0005] [0006] This method will add a metal catalyst, which will generate additional solid waste. The equipment requirements for decompression and water separation are complex, and the a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D239/06
CPCC07D239/06
Inventor 刘立强周鹏辉孟文斌王兵钱佐阵刘晓峰
Owner XIAN WONDER SCI & TECH
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