Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Process for synthesis of sodium glycididazole

A technology of sodium glycidazole and glycidazole is applied in the field of medicinal chemistry, and can solve the problems of mother liquor treatment, difficulty in recovery, unpleasant smell, and high pyridine unit consumption.

Inactive Publication Date: 2007-10-10
SHANDONG LUYE PHARMA CO LTD
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] (1) pyridine is highly toxic, volatile, and has an unpleasant smell, and it is difficult to process and recycle the mother liquor after the reaction;
[0011] (2) The unit consumption of pyridine is higher

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Process for synthesis of sodium glycididazole
  • Process for synthesis of sodium glycididazole
  • Process for synthesis of sodium glycididazole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0145] Embodiment 1, the preparation-esterification reaction of glycidiazole

[0146] A, in 100 liters of reactors, add 6.0 kilograms of nitrilotriacetic acid (1, 31.4mol), 30 kilograms of DMF and 12 kilograms of acetic anhydride (118mol), in 50 ℃ of insulated stirring reactions 6 hours;

[0147] B, add 14.0 kilograms (81.8mol) of metronidazole in the reactor, continue to insulate and stir the reaction for 7 hours at 40°C;

[0148] C. After the reaction is over, the interlayer passes cold water to cool the reaction feed liquid;

[0149] D. Cool the reaction liquid to 30°C, add purified water, stir until a precipitate precipitates out, and cool it down (<5°C) to precipitate crystals;

[0150] E. The precipitate is dried and dehydrated, washed with water until neutral;

[0151] F. After centrifugation, the crude product of glycididazole was obtained, with a wet weight of 9.18 kg and a yield of 47.0%.

Embodiment 2

[0152] Embodiment 2, the preparation-esterification reaction of glycidiazole

[0153] A, add 7.0 kilograms of nitrilotriacetic acid (1, 36.6mol), 30 kilograms of DMF and 16 kilograms of acetic anhydride (157mol) in 100 liters of reactors, in 65 ℃ of insulated stirring reactions 4 hours;

[0154] B, add 18.0 kilograms (105mol) of metronidazole in the reaction kettle, continue insulated stirring reaction at 60 ℃ for 5 hours;

[0155] C. After the reaction is over, the interlayer passes cold water to cool the reaction feed liquid;

[0156] D. Cool the reaction liquid to 30°C, add purified water, stir until a precipitate precipitates out, and cool it down (<5°C) to precipitate crystals;

[0157] E. The precipitate is dried and dehydrated, washed with water until neutral;

[0158] F. After centrifugation, the crude product of glycididazole was obtained, with a wet weight of 11.3 kg and a yield of 49.6%.

Embodiment 3

[0159] Embodiment 3, the preparation-esterification reaction of glycidiazole

[0160] A, add 8.0 kilograms of nitrilotriacetic acid (1, 41.8mol), 30 kilograms of DMF and 20 kilograms of acetic anhydride (196mol) in 100 liters of reactors, in 80 ℃ of insulated stirring reactions 2 hours;

[0161] B, add 22.0 kilograms (128mol) of metronidazole in the reactor, continue to insulate and stir the reaction for 3 hours at 80°C;

[0162] C. After the reaction is over, the interlayer passes cold water to cool the reaction feed liquid;

[0163] D. Cool the reaction liquid to 30°C, add purified water, stir until a precipitate precipitates out, and cool it down (<5°C) to precipitate crystals;

[0164] E. The precipitate is dried and dehydrated, washed with water until neutral;

[0165] F. After centrifugation, the crude product of glycididazole was obtained, with a wet weight of 13.4 kg and a yield of 51.4%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

This invention belongs to medicine chemical technology field. This invention discloses a new synthesis technique of dry ammonia double azole natrium. The material is nitrilotriacetic acid, then it reacts with acetic anhydride in N, N-dimethyl amide, and product is got after refining and salifying with bicarbonates. The reaction yield is high, cost is low of this technique, labor intensity is reduced, and it is convenient to scale producing and environment protection.

Description

Technical field: [0001] The invention belongs to the technical field of medicinal chemistry. Specifically relates to a synthesis process of glycidiazole sodium. Background technique: [0002] Cancer is a disease with high morbidity and mortality in the world, which seriously threatens human life. Tumor treatment is still dominated by surgery, radiotherapy and chemotherapy. In recent years, tumor radiotherapy patients are increasing day by day. However, the effect of tumor radiotherapy is not ideal. Even if the maximum possible radiation dose is used or the radiation method is changed, sometimes the radical cure cannot be achieved. [0003] Since the study of radiosensitizers began in the late 1950s, various types of compounds have been studied. Among them, more electrophilic compounds are studied. British Adams synthesized a series of nitroimidazole compounds from the analysis of electrophile theory and structure-activity relationship. The imizinidazole (MISO) screened o...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07D233/91
Inventor 宣坚钢吴蓉蓉莫道明代朝阳
Owner SHANDONG LUYE PHARMA CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com