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Method for preparing pharmaceutical intermediate 4(H) quinnazolidone

A manufacturing method, the technology of quinazolones, which is applied in the field of manufacturing the pharmaceutical intermediate 4 quinazolones, can solve problems such as declining profit margins, and achieve the effects of reducing volatilization and inhibiting reverse reactions

Inactive Publication Date: 2012-04-04
JIANGSU HAOHUA FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, the update speed of pharmaceutical intermediate products is fast, and the profit rate of a product will drop sharply after 3 to 5 years after it is generally launched on the market. This forces companies to continuously develop new products or continuously improve production processes in order to maintain high production profits.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] (1) 1644 kilograms of o-dichlorobenzene are dropped into the reaction kettle equipped with a water separator, and the N is passed for 2 minutes. 2 , put 548 kg of anthranilic acid and 180 kg of formamide at 25-30 ° C, and stir at 25-30 ° C for 10 minutes, pass N 2 10 minutes;

[0016] (2) Stir and heat up to 50±2°C for 1h, then slowly raise the temperature to 80±2°C for 3h, and collect the water generated by the reaction through the water separator, then raise the temperature to 120±2°C for 4h, and finally raise the temperature to 140±2°C Insulate at 2°C for 4 hours, and the reaction is complete when the collected water is 144 kg;

[0017] (3) Cool down to 25-28°C, discharge and centrifuge, mother liquor is 1574 kg, and the wet weight of crude product is 635 kg, put the crude wet product into the decolorization kettle, add 2500 kg of distilled water to heat up and reflux, and collect o-dichlorobenzene through the water separator 62 kg, until the steamed water is clear...

Embodiment 2

[0021] (1) 1711 kilograms of ortho-dichlorobenzene mother liquor and 70 kilograms of fresh ortho-dichlorobenzene are put into the reaction kettle that is equipped with water distributor, and logical 2 minutes N 2 , put 548 kg of anthranilic acid and 180 kg of formamide at 25-30 ° C, and stir at 25-30 ° C for 10 minutes, pass N 2 10 minutes;

[0022] (2) Stir and heat up to 50±2°C for 1h, then slowly raise the temperature to 80±2°C for 3h, and collect the water generated by the reaction through the water separator, then raise the temperature to 120±2°C for 4h, and finally raise the temperature to 140±2°C Insulate at 2°C for 4 hours, and the reaction is complete when the collected water is 144 kg;

[0023] (3) Cool down to 25-28°C, discharge and centrifuge to obtain a crude product with a wet weight of 639 kg and a mother liquor of 1718 kg. Put the crude wet product into a decolorization kettle, add 2425 kg of crystallization mother liquor and 75 kg of distilled water, heat up ...

Embodiment 3

[0027] (1) 1848 kilograms of ortho-dichlorobenzene mother liquor and 70 kilograms of fresh ortho-dichlorobenzene are put into the reaction kettle that is equipped with water separator, and logical 2 minutes N 2 , put 548 kg of anthranilic acid and 180 kg of formamide at 25-30 ° C, and stir at 25-30 ° C for 10 minutes, pass N 2 10 minutes;

[0028] (2) Stir and heat up to 50±2°C for 1h, then slowly raise the temperature to 80±2°C for 3h, and collect the water generated by the reaction through the water separator, then raise the temperature to 120±2°C for 4h, and finally raise the temperature to 140±2°C Insulate at 2°C for 4 hours, and the reaction is complete when the collected water is 144 kg;

[0029] (3) Cool down to 25-28°C, discharge and centrifuge to obtain 638 kg of crude product wet weight, recover 1852 kg of mother liquor, put the crude wet product into the decolorization kettle, add 2425 kg of crystallization mother liquor and 75 kg of distilled water, heat up and re...

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PUM

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Abstract

The invention discloses a method for preparing pharmaceutical intermediate 4(H) quinnazolidone, which comprises the following steps of: dissolving ortho-aminobenzoic acid and formamide in an inert solvent of o-dichlorobenzene; performing heat preservation reaction by steps under the protection of nitrogen, namely performing intermolecular condensation reaction and then intramolecular cyclization reaction; meanwhile, removing water generated in the process of reaction in time by using a water knockout trap to ensure that the positive reaction is performed smoothly; and decoloring, crystallizing and drying to obtain an ultimate product, namely the 4(H) quinnazolidone, wherein the mass ratio of the o-dichlorobenzene to the ortho-aminobenzoic acid is 3.0-3.5:1; the molar ratio of the ortho-aminobenzoic acid to the formamide is 1:1; and when the heat preservation reaction is performed by steps, the heat is preserved at the temperature of 50+ / -2 DEG C for 1 hour, 80+ / -2 DEG C for 3 hours, 120+ / -2 DEG C for 4 hours and 140+ / -2 DEG C for 4 hours. The preparation method has the advantages of simple process, zero emission, energy conservation, environmental protection and capacity of ensuring the quality and the yield of the product.

Description

technical field [0001] The present invention relates to the manufacturing method of cardiovascular and cerebrovascular pharmaceutical intermediates, in particular to the manufacturing method of pharmaceutical intermediate 4(H) quinazolones. technical background [0002] At present, my country needs more than 2,000 kinds of raw materials and intermediates for chemical industry every year, with a demand of more than 2.5 million tons. After more than 30 years of development, the chemical raw materials and intermediates required for my country's pharmaceutical production can basically be matched, and only a small part needs to be imported. And because our country is relatively rich in resources and the price of raw materials is low, many intermediates have been exported in large quantities. [0003] However, the update speed of pharmaceutical intermediate products is fast, and the profit rate of a product will drop sharply after 3 to 5 years after it is generally launched on th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/88
Inventor 吴昊万学明
Owner JIANGSU HAOHUA FINE CHEM
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