Synthetic method for organically compounding intermediate cyanogen

A technology for the synthesis of ethanedinitrile and a synthetic method, which is applied in the field of synthesis of the organic synthesis intermediate ethanedinitrile, can solve the problems of low final yield and complicated process, shorten the reaction time, reduce intermediate links, and improve the reaction rate. Yield effect

Inactive Publication Date: 2018-07-10
CHENGDU DONG DIAN AI ER TECH
0 Cites 0 Cited by

AI-Extracted Technical Summary

Problems solved by technology

However, most of the existing synthetic methods use sodium cyanide as the reactant, the process is more complicated, and the final yield is not very high. Therefore, it is necessary to ...
View more

Abstract

Provided is a synthetic method for organically compounding intermediate cyanogen. The method mainly comprises the following steps that 5 moles of 1,4-diiodobutane dissolves in 5 liters of acetone solution, the stirring speed is controlled at 110-150 revolutions per minute, 6-7 moles of 4-methyl-benzonitrile is added into, the temperature of the solution is heated to 60-70 DEG C, circulation refluxis carried out for 90-110 minutes, the temperature of the solution is reduced to 10-15 DEG C, filtering is carried out, a filter mass is washed by a methylamine solution, and then poured into a potassium iodide solution, stratification occurs, an oil layer is washed by a sodium chloride solution, pentane solution and ethyl acetate solution in sequence, reduced pressure distillation is carried out, cut fraction of 50-55 DEG C is collected, dehydration is carried out by using a dehydrating agent, and finished cyanogen is obtained.

Application Domain

Carboxylic acid nitrile preparationOrganic compound preparation

Technology Topic

Revolutions per minuteBenzonitrile +12

Image

  • Synthetic method for organically compounding intermediate cyanogen

Examples

  • Experimental program(3)

Example Embodiment

[0010] Example 1:
[0011] Dissolve 5mol of 1,4-diiodobutane in 5L of 30% acetone solution, control the stirring speed at 110rpm, add 6mol of 4-methyl-benzonitrile, raise the temperature of the solution to 60℃, and reflux for 90min , Reduce the temperature of the solution to 10℃, filter, wash the filter cake with 50% methylamine solution with mass fraction, pour into 20% potassium iodide solution with mass fraction, and the oil layer should be washed with sodium chloride solution, mass fraction is 70% Washing with pentane solution, washing with 80% ethyl acetate solution with mass fraction, 30kPa vacuum distillation, collecting 50°C fractions, dehydrating with anhydrous sodium sulfate dehydrating agent, to obtain 480.6g of finished oxonitrile with a yield of 89%.

Example Embodiment

[0012] Example 2:
[0013] Dissolve 5mol of 1,4-diiodobutane in 5L of 32% acetone solution, control the stirring speed to 130rpm, add 6.5mol of 4-methyl-benzonitrile, raise the temperature of the solution to 65℃, and reflux 100min, reduce the temperature of the solution to 12℃, filter, wash the filter cake with a mass fraction of 52% methylamine solution, pour into a 23% potassium iodide solution, and then layer the oil layer with sodium chloride solution, the mass fraction is 72 Wash with %pentane solution, wash with 82% ethyl acetate solution, 35kPa vacuum distillation, collect the 52°C distillate, and dehydrate with anhydrous potassium carbonate dehydrating agent to obtain 491.4g of finished oxonitrile with a yield of 91%.

Example Embodiment

[0014] Example 3:
[0015] Dissolve 5mol of 1,4-diiodobutane in 5L of 35% acetone solution, control the stirring speed at 150rpm, add 7mol of 4-methyl-benzonitrile, raise the temperature of the solution to 70℃, and reflux for 110min , Reduce the temperature of the solution to 15℃, filter, wash the filter cake with a 55% mass fraction of methylamine solution, pour into a 27% mass fraction of potassium iodide solution, layering occurs, and wash the oil layer with sodium chloride solution, with a mass fraction of 75% Washing with pentane solution, washing with 85% ethyl acetate solution with mass fraction, 40kPa vacuum distillation, collecting 55°C distillate, dehydrating with anhydrous sodium sulfate dehydrating agent, to obtain 507.6g of finished oxonitrile with a yield of 94%.

PUM

no PUM

Description & Claims & Application Information

We can also present the details of the Description, Claims and Application information to help users get a comprehensive understanding of the technical details of the patent, such as background art, summary of invention, brief description of drawings, description of embodiments, and other original content. On the other hand, users can also determine the specific scope of protection of the technology through the list of claims; as well as understand the changes in the life cycle of the technology with the presentation of the patent timeline. Login to view more.

Similar technology patents

Second harmonic type power grid synchronous frequency-locked loop method

ActiveCN113447715AReduce intermediate linksreduce mistakes
Owner:YANSHAN UNIV

Method for synthesis of haloperidol drug intermediate 4-chlorobutyronitrile

InactiveCN105503650AReduce intermediate linksReduce reaction temperature and reaction time
Owner:CHENGDU QIANYE LONGHUA PETROLEUM ENG TECH CONSULTING

Pharmaceutical intermediate 2,4-difluorobenzoic acid synthesis method

InactiveCN108623447AReduce intermediate linksshort reaction time
Owner:CHENGDU ZHONGHENG HUATIE TECH CO LTD

Special grinding wheel for liquid crystal glass

InactiveCN103331705AImprove conductivityReduce intermediate links
Owner:镇江丰成特种工具有限公司

Precise hemodialysis system

PendingCN112843361AReduce intermediate links
Owner:江苏关怀医疗科技有限公司

Classification and recommendation of technical efficacy words

  • short reaction time
  • Reduce intermediate links

High-concentration fast preparation method for silver nanowires

InactiveCN101934378Ashort reaction timeImprove reaction efficiency and equipment utilization
Owner:ZHEJIANG UNIV

Method for on-line synthesizing glucose-6-palmitate by lipase catalysis

ActiveCN103184249Ashort reaction timeHigh reaction selectivity and conversion
Owner:ZHEJIANG UNIV OF TECH

Method for synthesizing dyestuff intermediate H acid by naphthalene

ActiveCN101717355AThe reaction steps are simpleshort reaction time
Owner:泰兴锦汇化工有限公司

Intermittent on-off type mass concrete cooling water supply control system

ActiveCN102864930AReduce intermediate linkssimple system
Owner:HUBEI GEZHOUBA TESTING +1

Enclosed heat radiation system of industry control computer

InactiveCN101436093AReduce intermediate linksImprove thermal efficiency
Owner:BEIJING EVOC INTELLIGENT TECH +1

After-treatment device and preparation method for hollow ultrafiltration membrane wires

ActiveCN106268360AReduce intermediate linksReduce middleware
Owner:BEIJING ORIGIN WATER FILM TECH

Operation and maintenance management system based on network topological structure

ActiveCN103973484AReduce intermediate linksImprove efficiency
Owner:SUNINFO INFORMATION TECH

Three-degree-of-freedom parallel ankle joint rehabilitation mechanism and control method thereof

InactiveCN110559159ASimple hardware structureReduce intermediate links
Owner:HOHAI UNIV CHANGZHOU
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