Halcinonide producing process

A production process, the technology of hascinide, which is applied in the field of production technology of fluorine on hascinide, can solve the problems of low quality and yield, prone to hydrolysis, strong solvent polarity, etc., and achieves enhanced selectivity and improved yield. rate and quality, the effect of reducing the content of impurities

Inactive Publication Date: 2004-03-17
天津药业集团有限公司
View PDF0 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its shortcoming is that water is used as a solvent, the polarity of the solvent is strong, and the selectivity of the reaction is not high. During the reaction, the 21-position is prone to hydrolysis, resulting in unstable reaction and low quality and yield.

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Use 12kg of the halcinonide intermediate to condense the ring; add 60kg of 60% hydrogen fluoride aqueous solution to carry out the fluorine reaction, after the reaction is completed, dilute in 1200L ice water, ammonia water, neutralize, filter, and dry; then carry out recrystallization and refinement, with a volume ratio of Dissolve in a 7:3 mixed solvent of chloroform and methanol; concentrate, then flush into methanol; recrystallize in methanol, filter, and dry to obtain 8.4kg of fluoride, with a melting point of 220°C.

Embodiment 2

[0018] Use 12kg of the halcinonide intermediate to condense the ring; add 60kg of 54% hydrogen fluoride and dimethylformamide mixed solution to carry out the fluorine reaction, after the reaction is completed, dilute it in 1200L of ice water, neutralize in ammonia water, filter, and dry; Refined crystallization, dissolved in a mixed solvent of chloroform and methanol with a volume ratio of 7:3; concentrated, washed into methanol at a later stage; recrystallized in methanol, filtered, and dried to obtain 8.9kg of fluorine compound with a melting point of 226°C.

Embodiment 3

[0020] Use 12kg of halcinonide intermediate condensation products; add 60kg of 58% hydrogen fluoride and dimethylformamide mixed solution to carry out the fluorine reaction, after the reaction is completed, dilute in 1200L ice water, ammonia water, neutralize, filter, and dry; Refined crystallization, dissolved in a mixed solvent of chloroform and methanol with a volume ratio of 7:3; concentrated, washed into methanol at a later stage; recrystallized in methanol, filtered, and dried to obtain 9kg of fluoride, melting point 228°C.

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

The present invention is the production process of fluorizing Halcinonide with intermediate condensating and reducing as material. The technological process incldues fluorizing reaction with hydrogen fluoride and dimethyl methane amide solution, dilution with great amount of water, neutralization with ammonia water, filtering, and drying; recrystallization to refine through dissolution with mixed solvent of chloroform and methanol, concentration, addition of methanol for recrystallization; and filtering and drying to obtain the fluorized Halcinonide product. The said technological process has high yield and quality of the fluorized product.

Description

Technical field: [0001] The invention relates to a production process of fluorine on halcinonide. Background technique: [0002] The traditional fluorine-encapsulating production process of halcinonide uses halcinonide intermediate condensate as a raw material, and uses 60% hydrogen fluoride aqueous solution to carry out fluorine-reaction. After the reaction is completed, it is diluted with a large amount of water, neutralized with ammonia water, filtered, and dried; Then carry out recrystallization and refinement, dissolve with a mixed solvent of chloroform and methanol with a volume ratio of 7:3; Its shortcoming is that water is used as a solvent, the polarity of the solvent is strong, the selectivity of the reaction is not high, and the 21-position is prone to hydrolysis during the reaction process, resulting in unstable reaction and low quality and yield. [0003] Condensation compound Fluorine compound Invention content: [0004] Aiming at the existing...

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): C07J7/00C07J71/00
Inventor 张宝安王福军倪红凯
Owner 天津药业集团有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap