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Method for synthesizing 1, 3-bi [3-(dimethylamino) propyl] urea

A dimethylamine-based and synthetic method technology is applied in the production field of urea derivatives, can solve the problems of increasing process requirements and equipment conditions, high vacuum degree requirements, limiting production capacity, etc., and achieves good protection effect, simple equipment and convenient use. and the effect of

Inactive Publication Date: 2019-06-28
HUBEI HECHANG NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the boiling point of 1,3-bis[3-(dimethylamino)propyl]urea is very high, and the vacuum degree required for vacuum distillation is high.
In this way, it not only increases the process requirements and equipment conditions, but also greatly increases the cost, and at the same time limits the production capacity
Therefore, this method is generally not suitable for large-scale preparation of 1,3-bis[3-(dimethylamino)propyl]urea

Method used

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  • Method for synthesizing 1, 3-bi [3-(dimethylamino) propyl] urea
  • Method for synthesizing 1, 3-bi [3-(dimethylamino) propyl] urea

Examples

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Embodiment 1

[0024] In the present embodiment, the synthetic method of 1,3-bis[3-(dimethylamino)propyl]urea is as follows:

[0025] Mix 4.38g of urea and 18.6g of N,N-dimethyl-1,3-propanediamine, add 0.5g of 85% hydrazine hydrate, heat up to 105-110°C, and gradually heat up to 130°C after reacting for 5-10min. After keeping for 1 hour, the temperature was raised to 150°C, and after keeping for 1 hour, the temperature was lowered to 30°C. Unreacted N,N-dimethyl-1,3-propanediamine was distilled off under reduced pressure to obtain a colorless and transparent viscous liquid product with a yield of 92.6% based on urea.

[0026] The target product of this example was analyzed by gas chromatography, and 1,3-bis[3-(dimethylamino)propyl]urea purchased from Shanghai Baishikai Chemical Technology Co., Ltd. was used as a standard for comparison. Under the same gas phase conditions, the peak time of the standard product is 1.337min, and the peak time of the target product in this embodiment is 1.332m...

Embodiment 2

[0028] In the present embodiment, the synthetic method of 1,3-bis[3-(dimethylamino)propyl]urea is as follows:

[0029] Mix 11.7g of urea and 38.7g of N,N-dimethyl-1,3-propanediamine, add 0.3g of semicarbazide hydrochloride and 0.1g of 85% hydrazine hydrate, raise the temperature to about 110°C, and gradually raise the temperature after reacting for 5-10min to 130°C, keep it for 1h, then raise the temperature to 150°C, keep it for 1h, then cool down to 30°C. Unreacted N,N-dimethyl-1,3-propanediamine was distilled off under reduced pressure to obtain a colorless and transparent viscous liquid product. The yield is 93.4% based on urea. The product contains 1.1% of the product in the form of chloride salt through liquid phase detection, and can be directly used in the synthesis of polyquaternium salt.

Embodiment 3

[0031] In the present embodiment, the synthetic method of 1,3-bis[3-(dimethylamino)propyl]urea is as follows:

[0032] Take 17.0g of urea and 66.84g of N,N-dimethyl-1,3-propanediamine, mix them, add 0.3g of carbohydrazide, raise the temperature to about 110°C, react for 5-10min, then gradually raise the temperature to 130°C, and keep it for 1h Then raise the temperature to 150°C, keep it for 1h and then cool down. Unreacted N,N-dimethyl-1,3-propanediamine was distilled off under reduced pressure to obtain a colorless and transparent viscous liquid product with a yield of 94.0% based on urea. The gas chromatographic analysis purity of the target product in this embodiment is greater than 98%.

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Abstract

The invention relates to a method for synthesizing 1, 3-bi [3-(dimethylamino) propyl] urea, which comprises the following steps: 1, taking urea and N, N-dimethyl-1, 3-propylene diamine and mixing in acertain ratio, adding a protective reagent, heating to 105-150 DEG C for reaction; wherein the protective agent is selected from one or more of hydrazine or hydrazine derivatives; 2, removing unreacted N, N-dimethyl-1, 3-propylenediamine to obtain the desired product 1, 3-bi [3-(dimethylamino) propyl] urea. The protective reagent slowly decomposes into a reducing ammonia gas under the reaction heating condition, protects the reaction product, and reduces the possibility of oxidation of the product. The synthesis method can directly obtain a colorless product without nitrogen protection, without further purification or refining, and the product can also be directly used as a raw material for further reaction. The method has low requirements on reaction conditions, simple equipment, and cansignificantly reduce the production cost of the target compound, and is suitable for producing a small amount and a large amount of 1, 3-bi [3-(dimethylamino) propyl] urea.

Description

technical field [0001] The invention relates to the technical field of production of urea derivatives, in particular to a synthesis method of 1,3-bis[3-(dimethylamino)propyl]urea. Background technique [0002] 1,3-bis[3-(dimethylamino)propyl]urea is a chemical substance in which the two amino groups of urea are replaced by amines, and it is a molecule with the following structure: [0003] [0004] 1,3-bis[3-(dimethylamino)propyl]urea is widely used in industries such as medicine, pesticides, dyes, electroplating intermediates, petrochemicals, semiconductor manufacturing and polymers, and is an important Fine organic chemical intermediates. For example, 1,3-bis[3-(dimethylamino)propyl]urea can be used to synthesize polyquaternary ammonium salts, which are widely used in the fields of daily chemicals, textiles, medicine, water treatment and electroplating, and can be used as high-performance Bactericide and algaecide, slime stripping agent, electroplating additive, can b...

Claims

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Application Information

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IPC IPC(8): C07C273/18C07C275/14
Inventor 隗兰华杨和平丁博叶楚平
Owner HUBEI HECHANG NEW MATERIAL TECH
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