Supercharge Your Innovation With Domain-Expert AI Agents!

Preparation method of methylene-cyclo methane-disulfonate

A technology of methylene disulfonate and methylene disulfonic acid, which is applied in the direction of organic chemistry, can solve the problems of low yield and no industrial value, and achieve high yield, low cost and mild reaction conditions Effect

Active Publication Date: 2013-11-06
SHIJIAZHUANG SAN TAI CHEM CO LTD
View PDF1 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] This process uses solid methylene disulfonic acid (must be solid) and paraformaldehyde as reaction raw materials, and reacts for 10 hours at 120°C to obtain MMDS, but the yield is relatively low, and the highest can only reach 50%.
no industrial value

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
  • Preparation method of methylene-cyclo methane-disulfonate
  • Preparation method of methylene-cyclo methane-disulfonate
  • Preparation method of methylene-cyclo methane-disulfonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The utensil used in the production of methylene disulfonate is a 500ml four-necked flask, which is equipped with a mechanical stirrer, a thermometer, and a dropping funnel. Put 18g of solid methylene disulfonic acid into a four-neck flask, heat up to 110°C, add 23.8g of acylating reagent thionyl chloride dropwise with a dropping funnel, keep the reaction for 6 hours after the dropwise addition, and then cool down to 0 ℃, reduced pressure (10mmHG) for 1 hour, and then raised the temperature to 120°C, then added 3.3 g of cyclization reagent paraformaldehyde to the four-necked flask, and reacted for 24 hours. After the reaction was completed and cooled to room temperature, the extraction solvent was added to the four-necked flask Extract three times with 200ml of chloroform, add 1g of activated carbon to the combined extract to reflux for decolorization for 1 hour, then suction filter, concentrate, and then quickly cool down to crystallize after concentration, the crystalli...

Embodiment 2

[0024] Put 18g of solid methylene disulfonic acid into a 500ml four-necked flask, heat up to 40°C, add 6.85g of acylating reagent phosphorus trichloride dropwise, keep this temperature after the dropwise addition, react for 9 hours, and then add Add 200ml of organic solvent dichloromethane into the bottle mouth, add 8g of methylal, continue to keep the temperature at 40°C for reflux reaction for 20 hours, after the reaction is completed, add 1g of activated carbon to reflux for decolorization for 1 hour, then suction filter, concentrate, and then gradient cooling crystallization after concentration , the crystallization temperature was at -10°C, the crystallization time was 6 hours, and then filtered, and after drying under reduced pressure, 14.3 g of white crystals of fine methylene disulfonate were obtained, with a yield of 76.1%. The nuclear magnetic spectrum was 1 H-NMR (400 MHz, CD3CN) δ (ppm): 5.33 (s, 2H), 6.00 (s, 2H).

[0025] In the above-mentioned reaction of the pr...

Embodiment 3

[0027] Add 300ml of chloroform into a 500ml four-necked flask, then add 18g of methylene disulfonic acid solid, raise the temperature to 62°C, add 10.4g of acylating reagent phosphorus pentachloride, and keep the reaction for 16 hours. After the reaction was completed, keep the temperature and then add 4 g of paraformaldehyde into the four-necked flask, and reflux for 10 hours. After the reaction is completed, add 1 g of activated carbon to reflux for decolorization for 1 hour, then filter with suction, concentrate, and then cool down to crystallize after concentration. The crystallization temperature is 0°C, and the crystallization time is 4 hours. 11.6g of white crystals of cyclomethylene acid, the yield is 61.7%, and the nuclear magnetic spectrum is 1 H-NMR (400 MHz, CD3CN) δ (ppm): 5.33 (s, 2H), 6.00 (s, 2H).

[0028] In the above-mentioned reaction of the present embodiment, the organic solvent can also be one or a mixture of dichloromethane, carbon tetrachloride, ethyl ...

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 discloses a preparation method of methylene-cyclo methane-disulfonate, belonging to the field of organic chemistry synthesis. The method comprises the following steps of: acylation reaction: carrying out an acylation reaction on methylene-disulfonic acid and an acylation agent to obtain a mixture containing methylene disulfonyl chloride; cyclization reaction: carrying out a cyclization reaction on the methylene disulfonyl chlorine or a mixture containing methylene disulfonyl chlorine and a cyclization agent to obtain a mixture containing methylene-cyclo methane-disulfonate; and separation and purification: separating and purifying the mixture containing methylene-cyclo methane-disulfonate. The method disclosed by the invention has the advantages of low cost, high product yield and high product quality.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and in particular relates to a preparation process of methylene disulfonate. Background technique [0002] Methylene disulfonate, English name 1,5,2,4-Dioxadithiane (MMDS for short), molecular formula C 2 h 4 o 6 S 2 , CAS: 99591-74-9 Structural formula: [0003] [0004] Methylene disulfonate is an important pharmaceutical intermediate and electronic chemical. The sulfonic acid group contained in the structure can react with alcohol, phenol, thiol and other groups under certain conditions, and its unique structure plays a huge role in the synthesis of heterocyclic drugs. In recent years, with the development of new energy technologies, the application of MMDS in lithium battery electrolyte additives has gradually been developed. MMDS is used in lithium battery electrolyte additives, which can significantly improve battery performance, increase battery recharge times and cycle characteri...

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): C07D327/00
Inventor 刘鹏梅银平
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

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

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com