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Synthesizing method of phthaloyl-beta-alanine

A technology of phthaloyl and phthalic anhydride, which is applied in the field of chemical synthesis, can solve the problems of complex operation control, high equipment requirements, complicated operation, etc., and achieves simple operation, high equipment utilization rate, and no use of solvents. Effect

Active Publication Date: 2011-05-04
石河子市郁茏生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The above two preparation methods of phthalyl-β-alanine, the first method adopts a conventional liquid phase reaction system, uses an organic solvent, complex operation, low yield, and pollutes the environment
The second method uses a melting reaction system, which requires high equipment, complicated operation and control, and high energy consumption.
There are no research reports on the preparation of phthalyl-β-alanine by microwave thermal effect and low-heat solid-state reaction at home and abroad

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 8.9g of β-alanine and 26.7mg of sodium carbonate, mix and grind thoroughly. Add 14.8 g of phthalic anhydride and 44.4 mg of sodium chloride, and grind thoroughly. The materials were put into a microwave reactor for reaction to obtain 22.4 g of the product with a purity of 99.7%.

[0030] The reaction conditions are as follows: microwave oscillation frequency: 600MHZ; microwave power: 600w; heating time: 30 minutes; heating temperature: 85°C.

Embodiment 2

[0032] Take 8.9g of β-alanine and 26.7mg of sodium carbonate, mix and grind thoroughly. Add 14.8 g of phthalic anhydride and 44.4 mg of sodium chloride, and grind thoroughly. The materials were put into a microwave reactor for reaction to obtain 22.0 g of the product with a purity of 99.4%.

[0033] The reaction conditions are as follows: microwave oscillation frequency: 900MHZ; microwave power: 600w; heating time: 30 minutes; heating temperature: 85°C.

Embodiment 3

[0035] Take 8.9g of β-alanine and 53.4mg of sodium carbonate, mix them and grind them thoroughly. Add 14.8 g of phthalic anhydride and 88.8 mg of sodium chloride, and grind thoroughly. The materials were put into a microwave reactor for reaction to obtain 22.5 g of the product with a purity of 99.6%.

[0036] The reaction conditions are as follows: microwave oscillation frequency: 600MHZ; microwave power: 600w; heating time: 30 minutes; heating temperature: 85°C.

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PUM

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Abstract

The invention discloses a synthesizing method of phthaloyl-beta-alanine. In the synthesizing method, the phthaloyl-beta-alanine is prepared through grinding and microwave irradiation by taking beta-alanine and phthalic anhydride as raw materials and sodium carbonate and sodium chloride as mineralizers. The synthesizing method has the advantages of high selectivity, thorough reaction, high yield, low energy consumption, little pollution, suitability for industrial production and wide prospect.

Description

technical field [0001] The invention relates to a synthesis method of a compound, in particular to a synthesis method of L-carnosine intermediate phthalyl-β-alanine, and belongs to the technical field of chemical synthesis. Background technique [0002] L-carnosine was first detected in beef by Russian scientists Gulewitsh and Amiradzibi in 1900, and it exists widely in mammalian brain, muscle and other tissues with nerve distribution. Its concentration in animals is about 1-20mmol / l. It is synthesized by carnosine synthase using β-alanine and L-histidine, and the main synthesis sites are muscle and brain. Because of its antioxidant properties, free radical scavenging, transition metal chelation, neuroprotection, wound healing promotion and anti-aging effects, carnosine has broad application prospects in the fields of medicine, health care, and hygiene. [0003] It has been reported in the literature that the common method for synthesizing L-carnosine is to use β-alanine a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/48
Inventor 姚成盛
Owner 石河子市郁茏生物科技有限公司
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