CN103804177A - Production process for synthesizing bromopyruvate - Google Patents
Production process for synthesizing bromopyruvate Download PDFInfo
- Publication number
- CN103804177A CN103804177A CN201410033254.3A CN201410033254A CN103804177A CN 103804177 A CN103804177 A CN 103804177A CN 201410033254 A CN201410033254 A CN 201410033254A CN 103804177 A CN103804177 A CN 103804177A
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- China
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- reaction
- bromopyruvate
- acetone acid
- bromine
- acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/347—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups
- C07C51/363—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups by introduction of halogen; by substitution of halogen atoms by other halogen atoms
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a production process for synthesizing bromopyruvate, relating to the technical field of chemical engineering. The production process comprises the steps of stirring pyruvic acid, a solvent and sulfuric acid for reaction, adding bromine for reaction, finishing reaction when a reaction liquid is changed to be colorless, removing the solvent in reactants to obtain crude bromopyruvate, using heated benzene for recrystallization, filtering, carrying out vacuum drying to obtain pure bromopyruvate, and then packaging and warehousing. The production process is simple and convenient, is environment-friendly and pollution-free, and is convenient to operate, and has low equipment investment and high purity, the raw materials are easily available, and the prepared bromopyruvate has a good using effect, safety and reliability.
Description
Technical field
The present invention relates to chemical technology field, be specifically related to the synthetic production technique of a kind of bromo acetone acid.
Background technology
Bromo acetone acid is burgundy or orange transparent liquid; Smell with irritating, density 1.561g/cm
3, boiling point: 224.3 ℃, specific refractory power: 1.4675-1.4765, flash-point: 75.4 ℃, vapour pressure: 0.0919mmHg, a kind of important chemical reagent of bromo acetone acid and intermediate.Purposes is comparatively extensive, can be used for the synthetic of dyestuff, fungicidal preservative etc., at present still more traditional mode of the method for industrial production bromo acetone acid, in this traditional production method, there is the problems such as yield is low, not high pollution of purity is serious, and production technique is comparatively complicated, is difficult to meet human wants.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of purity high, the production technique that the simple bromo acetone acid of preparation technology is synthetic.
Technical problem to be solved by this invention realizes by the following technical solutions:
The production technique that bromo acetone acid is synthetic, is characterized in that: comprise following processing step,
A. choose a 100ml there-necked flask and be 98.5% pyruvic acid, the solvent of 25-35ml and the sulfuric acid that 0.05-0.1g purity is 98.0% to adding 4.5-5g purity in there-necked flask, open and stir, and temperature in flask is controlled to 40-50 ℃.
B. take 9-10g bromine, and bromine is adopted to vitriol oil washing, then the bromine after washing is added in the there-necked flask in step a and is reacted.
C. adopt air to replace the Hydrogen bromide generating in reaction process in step b.
D. after reactant reaction 2.0-4.0h in above-mentioned steps b, cool the temperature to 0 ℃ of then standing 3.0-4.0h of holding temperature.
E. become colorless after liquid until the reaction liquid of above-mentioned reactant, be considered as reaction and finish, after the solvent in reactant is dispelled, obtain bromo acetone acid crude product.
F. adopt the benzene after heating to carry out recrystallization above-mentioned crude product bromo acetone acid, then filter rear employing vacuum-drying and obtain sterling bromo acetone acid, then pack warehouse-in.
The invention has the beneficial effects as follows: the present invention is easy to prepare simple, and environment friendly and pollution-free, raw material is easy to get, and facility investment is few, and purity is high, convenient operation, the bromo acetone acid result of use of preparation is good, safe and reliable.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach object and effect is easy to understand, below in conjunction with specific embodiment, further set forth the present invention.
Embodiment 1
The production technique that bromo acetone acid is synthetic, comprises following processing step,
A. choose a 100ml there-necked flask and be 98.5% pyruvic acid, the solvent of 25ml and the sulfuric acid that 0.05g purity is 98.0% to adding 4.5g purity in there-necked flask, open and stir, and temperature in flask is controlled to 40 ℃.
B. take 9g bromine, and bromine is adopted to vitriol oil washing, then the bromine after washing is added in the there-necked flask in step a and is reacted.
C. adopt air to replace the Hydrogen bromide generating in reaction process in step b.
D. after reactant reaction 2.0h in above-mentioned steps b, cool the temperature to 0 ℃ of then standing 3.0h of holding temperature.
E. become colorless after liquid until the reaction liquid of above-mentioned reactant, be considered as reaction and finish, after the solvent in reactant is dispelled, obtain bromo acetone acid crude product.
F. adopt the benzene after heating to carry out recrystallization above-mentioned crude product bromo acetone acid, then filter rear employing vacuum-drying and obtain sterling bromo acetone acid, then pack warehouse-in.
Embodiment 2
The production technique that bromo acetone acid is synthetic, comprises following processing step,
A. choose a 100ml there-necked flask and be 98.5% pyruvic acid, the solvent of 30ml and the sulfuric acid that 0.07g purity is 98.0% to adding 4.9g purity in there-necked flask, open and stir, and temperature in flask is controlled to 45 ℃.
B. take 9.4g bromine, and bromine is adopted to vitriol oil washing, then the bromine after washing is added in the there-necked flask in step a and is reacted.
C. adopt air to replace the Hydrogen bromide generating in reaction process in step b.
D. after reactant reaction 3.0h in above-mentioned steps b, cool the temperature to 0 ℃ of then standing 3.5h of holding temperature.
E. become colorless after liquid until the reaction liquid of above-mentioned reactant, be considered as reaction and finish, after the solvent in reactant is dispelled, obtain bromo acetone acid crude product.
F. adopt the benzene after heating to carry out recrystallization above-mentioned crude product bromo acetone acid, then filter rear employing vacuum-drying and obtain sterling bromo acetone acid, then pack warehouse-in.
More than show and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (1)
1. the synthetic production technique of bromo acetone acid, is characterized in that: comprise following processing step,
A. choose a 100ml there-necked flask and be 98.5% pyruvic acid, the solvent of 25-35ml and the sulfuric acid that 0.05-0.1g purity is 98.0% to adding 4.5-5g purity in there-necked flask, open and stir, and temperature in flask is controlled to 40-50 ℃.
B. take 9-10g bromine, and bromine is adopted to vitriol oil washing, then the bromine after washing is added in the there-necked flask in step a and is reacted.
C. adopt air to replace the Hydrogen bromide generating in reaction process in step b.
D. after reactant reaction 2.0-4.0h in above-mentioned steps b, cool the temperature to 0 ℃ of then standing 3.0-4.0h of holding temperature.
E. become colorless after liquid until the reaction liquid of above-mentioned reactant, be considered as reaction and finish, after the solvent in reactant is dispelled, obtain bromo acetone acid crude product.
F. adopt the benzene after heating to carry out recrystallization above-mentioned crude product bromo acetone acid, then filter rear employing vacuum-drying and obtain sterling bromo acetone acid, then pack warehouse-in.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410033254.3A CN103804177A (en) | 2014-01-23 | 2014-01-23 | Production process for synthesizing bromopyruvate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410033254.3A CN103804177A (en) | 2014-01-23 | 2014-01-23 | Production process for synthesizing bromopyruvate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103804177A true CN103804177A (en) | 2014-05-21 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410033254.3A Pending CN103804177A (en) | 2014-01-23 | 2014-01-23 | Production process for synthesizing bromopyruvate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103804177A (en) |
-
2014
- 2014-01-23 CN CN201410033254.3A patent/CN103804177A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 汪烈焰等: "溴代丙酮酸的合成研究", 《精细化工》 * |
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Application publication date: 20140521 |