Method for preparing florfenicol intermediate salt

A florfenicol and intermediate technology, which is applied in the field of preparation of florfenicol intermediate salts, can solve the problems of difficult recovery of glycerol, large amount of sewage and high cost, and achieves good product quality, convenient operation and mild reaction conditions. Effect

Active Publication Date: 2012-01-18
XINCHANG HEBAO BIOTECH
View PDF3 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This technology makes producing certain chemical products more efficiently by avoiding complex processes or reactions that are harmful to our environment. It also reduces costs compared to existing methods while maintaining good yields over time. By mixing two different types of liquids together under specific temperature ranges (approximately 60 degrees Celsius), we can achieve high-yield production without causing damage from heat exposure during processing.

Problems solved by technology

Technological Problem addressed during this patented study describes how flufenoxicin can be prepared from certain chemical compounds that are commonly found naturally occurring substances called fluofensins or related molecules like fenflurazim. However, current methods have drawbacks including difficulty recovering excessive amounts of waste water produced after each step due to complicated processes involved with reductant production.

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
  • Method for preparing florfenicol intermediate salt
  • Method for preparing florfenicol intermediate salt
  • Method for preparing florfenicol intermediate salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In the three-necked flask, add 300g (9.36mol) methanol, 50g (0.17mol) D-threo-p-methylsulfonylphenylserine ethyl ester, raise the temperature to 35°C, add 13g (0.24mol) potassium borohydride, and keep warm for 5 hours , then add 50g (0.41mol) concentrated hydrochloric acid to adjust the pH to 3-3.5, keep warm at 75-80°C for 2-2.5 hours, distill off methanol and boron ester, adjust the pH of the residue to 7-7.5 with potassium hydroxide, spray dry, The hydrochloride product of the reduced product of the formula was 49.03 grams, the yield was 100%, the fixed nitrogen content was 4.90%, and the mp (melting point) was 152-154°C.

Embodiment 2

[0024] In the three-necked flask, add 300g (9.36mol) methanol, 50g (0.17mol) D-threo-p-methylsulfonylphenylserine ethyl ester, raise the temperature to 35°C, add 13g (0.24mol) potassium borohydride, and keep warm for 5 hours , then add 30g (0.311mol) of sulfuric acid to adjust the pH to 1-1.5, keep it warm at 50-55°C for 1-1.5 hours, evaporate methanol and boron ester, adjust the pH of the residue to 6-6.5 with sodium hydroxide, and evaporate to dryness under reduced pressure , to obtain 51.22 g of the reduced sulfate product, with a yield of 100%, a fixed nitrogen content of 4.76%, and mp160-163°C.

Embodiment 3

[0026] In the three-necked flask, add 300g (9.36mol) methanol, 50g (0.17mol) D-threo-p-methylsulfonylphenylserine ethyl ester, raise the temperature to 35°C, add 13g (0.24mol) potassium borohydride, and keep warm for 5 hours , and then add 34g (0.301mol) of phosphoric acid to adjust the pH to 1.5-2, keep the temperature at 60-65°C for 3.5-4 hours, evaporate methanol and boron ester, adjust the pH of the residue to 8.5-9.0 with sodium methoxide, and evaporate to dryness under reduced pressure. 50.98 g of the reduced phosphate product was obtained, with a yield of 99.53%, a fixed nitrogen content of 4.74%, and an mp of 155-157°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 invention provides a method for preparing a florfenicol intermediate salt, which comprises the following steps of: with D-threo-methylsulfonylphenylserine ethyl in a formula II shown in the specification and potassium borohydride as raw materials and methanol as a solvent, reacting at 35 DEG C for 5 hours; adjusting a pH value to acidity with acid; preserving the temperature for a period of time at heat preservation temperature; distilling; adjusting residues with alkali; and drying to obtain the target compound florfenicol intermediate salt in a formula III shown in the specification. The invention has the advantages that: the process is simple, reaction conditions are mild, is the yield is improved by 2-3 percent higher than that of the relevant document report, the cost is reduced by 1-2 percent lower than that the document report, the used raw materials can not cause environmental pollution, and the like.

Description

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

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
Owner XINCHANG HEBAO BIOTECH
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