CN106946693A - The preparation method of forensic science qualitative, quantitative Fratol - Google Patents
The preparation method of forensic science qualitative, quantitative Fratol Download PDFInfo
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- CN106946693A CN106946693A CN201710270296.2A CN201710270296A CN106946693A CN 106946693 A CN106946693 A CN 106946693A CN 201710270296 A CN201710270296 A CN 201710270296A CN 106946693 A CN106946693 A CN 106946693A
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- C07—ORGANIC CHEMISTRY
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- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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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
- C07C51/02—Preparation of carboxylic acids or their salts, halides or anhydrides from salts of carboxylic acids
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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
- C07C51/09—Preparation of carboxylic acids or their salts, halides or anhydrides from carboxylic acid esters or lactones
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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
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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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
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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Abstract
The preparation method of open court's science qualitative, quantitative Fratol of the present invention, comprises the following steps：(I) thick Fratol is prepared；(II) fluoroacetic acid is prepared；(III) pure Fratol is prepared：Fluoroacetic acid will be obtained and be dissolved in second alcohol and water according to volume ratio 10:In 1 mixed solution being made into, then saturation sodium hydroxide solution is added dropwise, the amount of the material of NaOH is 1.05 1.10 times of the amount of fluoroacetic acid material in mixed solution in the saturation sodium hydroxide solution added, and stirring is drying to obtain pure Fratol after filtering.The preparation method yield of forensic science qualitative, quantitative Fratol of the present invention is high, and the fluoroacetic acid purity prepared is high, can be used directly as standard items or reference material, meets in reality the need for forensic science toxicological analysis.
Description
Technical field
The present invention relates to forensic science toxicological analysis field.More particularly, to a kind of forensic science toxicological analysis field
Fluoroacetic acid preparation method.
Background technology
Because the toxicity of Fratol is huge, sale was forbidden by relevant department in 2003；But, because it is in agriculture
Industry production in kill mouse effect substantially, it is still on sale on the stall with goods spread out on the ground for sale of in the market especially rural market, thus caused homicide and from
Case is killed still to exist.In order to which this kind of poisonous substance whether there is in precise Identification body, it is necessary to determined using standard items or reference material
Property is quantitatively detected；However, the standard items of both the above material can not be bought from market, in order to meet forensic science field fluoroacetic acid
The test sensitivity of sodium and fluoroacetic acid Poisoning Cases, be badly in need of laboratory it is synthetically prepared go out forensic science toxicological analysis field fluorine
Sodium acetate and fluoroacetic acid.
The content of the invention
It is an object of the present invention to provide a kind of preparation method of forensic science qualitative, quantitative Fratol, in reality
Test preparation under the conditions of room so that the fluoroacetic acid prepared can be used directly as standard items or reference material, meet method in reality
The need for the science toxicological analysis of front yard.
To reach above-mentioned purpose, the present invention uses following technical proposals：The system of forensic science qualitative, quantitative Fratol
Preparation Method, comprises the following steps：(I) thick Fratol is prepared；(II) fluoroacetic acid is prepared；(III) pure Fratol is prepared：Will
Second alcohol and water is dissolved according to volume ratio 10 to fluoroacetic acid:In 1 mixed solution being made into, saturation NaOH is then added dropwise molten
The amount of the material of NaOH is the amount of fluoroacetic acid material in mixed solution in liquid, the saturation sodium hydroxide solution added
1.05-1.10 times, stirring is drying to obtain pure Fratol after filtering.
The preparation method of above-mentioned forensic science qualitative, quantitative Fratol, step (I) comprise the following steps：(1-1) will
Ethyl fluoroacetate or methylfluoracetate dissolving, be made solute for the ethyl fluoroacetate solution of ethyl fluoroacetate or methylfluoracetate or
Methylfluoracetate solution；(1-2) adds alkali into ethyl fluoroacetate solution or methylfluoracetate solution, stirring；(1-3) is filtered,
Filter residue is thick Fratol.
The preparation method of above-mentioned forensic science qualitative, quantitative Fratol, in step (1-1)：By ethyl fluoroacetate or
Methylfluoracetate is dissolved in alcohol, and the volume ratio of solute and solvent is (2-3)：40.
The preparation method of above-mentioned forensic science qualitative, quantitative Fratol, in step (1-1)：Alcohol be methanol, ethanol,
Any one or more in isopropanol and n-butanol.
The preparation method of above-mentioned forensic science qualitative, quantitative Fratol, in step (1-2)：It is molten to ethyl fluoroacetate
Alkali is added in liquid or methylfluoracetate solution, the addition of alkali is the amount of ethyl fluoroacetate or the material of methylfluoracetate
1.05-1.5 times.
The preparation method of above-mentioned forensic science qualitative, quantitative Fratol, in step (1-2)：Alkali be NaOH or
Potassium hydroxide, is stirred 10-20 hours, generates white depositions, and vacuum distillation obtains thick Fratol except solvent is to dry；In step
In (1-3), the thick Fratol solid of gained is washed with methyl tertiary butyl ether(MTBE), removes organic impurities and the complete raw material of unreacted, is done
It is dry.
The preparation method of above-mentioned forensic science qualitative, quantitative Fratol, step (II) comprise the following steps：(2-1) will
Thick Fratol is dissolved in acid solution；(2-2) uses Solvent Extract methods；(2-3) is filtered to remove magnesium sulfate, is by filtrate distillation
Obtain fluoroacetic acid.
The preparation method of above-mentioned forensic science qualitative, quantitative Fratol, in step (2-1)：Acid solution be hydrochloric acid or
Sulfuric acid, and with corresponding sodium salt or sylvite saturation；Organic solvent is ether or methyl tertiary butyl ether(MTBE) in step (2-2), is extracted
After isolate organic layer, and add anhydrous magnesium sulfate in organic layer and dry, overnight.
The preparation method of above-mentioned forensic science qualitative, quantitative Fratol, comprises the following steps：(I) thick fluoroacetic acid is prepared
Sodium；
141mmol, 13.6mL ethyl fluoroacetate or methylfluoracetate are dissolved in 240mL ethanol by (1-1)；
(1-2) adds 155mmol, 6.2g NaOH, and 12 hours are stirred at 50 c, generates white depositions；
(1-3) vacuum distillation obtains thick Fratol solid, the thick Fratol solid of gained is used respectively except solvent is to dry
30mL methyl tertiary butyl ether(MTBE)s are washed three times, remove organic impurities and the complete raw material of unreacted, are dried；
(II) fluoroacetic acid is prepared；
Thick Fratol is added in the hydrochloric acid that HCl concentration is 3mol/L by (2-1), and regulation solution ph is 4, and is added
NaCl is to saturation；
(2-2) is extracted 4 times with 100mL methyl tertiary butyl ether(MTBE)s respectively, merges organic phase, the anhydrous MgSO of organic layer4Dry,
Overnight；
Filtrate is distilled after (2-3) filtering, obtains 137mmol, 10.7g fluoroacetic acid.
Beneficial effects of the present invention are as follows：
1st, forensic science qualitative, quantitative of the present invention can be prepared in laboratory conditions with the preparation method of Fratol, production
Rate is high, and the fluoroacetic acid purity prepared is high, can be used directly as standard items (purity more than 99.5%) or reference material,
Meet in reality the need for forensic science toxicological analysis.
2nd, use single alcohol as solvent in hydrolysis, be easy to subsequent recovery to utilize.
3rd, the addition of alkali is moderate, in order to avoid in excessive Fratol of taking too much, and the too many acid of consumption is neutralized below.
4th, 50 DEG C of reaction temperatures for generating Fratol as being reacted with alkali are selected, can effectively shorten the reaction time.
5th, the thick Fratol organic solvent washing of gained, removes unreacted thoroughly raw material and other organic impurities, protects
The purity of final Fratol is demonstrate,proved, while the complete raw material of unreacted can also recycle and reuse.
6th, it is 4 with salt acid for adjusting pH, is easy to control the amount of hydrochloric acid, also ensures that fluoroacetic acid is tried one's best whole precipitations, improve simultaneously
Purity and yield.
7th, selection methyl tertiary butyl ether(MTBE) is as extractant, the advantage for making full use of methyl tertiary butyl ether(MTBE) boiling point high, industry
On it is more easy to operate, security is good.
8th, fluoroacetic acid is dissolved in second alcohol and water according to volume ratio 10:In 1 mixed solution being made into so that fluoroacetic acid can be suitable
Sharply Fratol is generated with NaOH reaction and all precipitated, it is ensured that the yield and purity of Fratol all compare
It is high.
Embodiment
Embodiment 1
The preparation method of forensic science qualitative, quantitative Fratol, comprises the following steps：(I) thick Fratol is prepared；
141mmol, 13.6mL ethyl fluoroacetate or methylfluoracetate are dissolved in 240mL ethanol by (1-1)；
(1-2) adds 155mmol, 6.2g NaOH, and 12 hours are stirred at 50 c, generates white depositions；
(1-3) decompression obtains thick Fratol solid, the thick Fratol solid of gained uses 30mL first respectively except solvent is to dry
Base tertbutyl ether is washed three times, removes organic impurities and the complete raw material of unreacted, is dried；
(II) fluoroacetic acid is prepared；
Thick Fratol is added in the hydrochloric acid that HCl concentration is 3mol/L by (2-1), and regulation solution ph is 4, and is added
NaCl is to saturation；
(2-2) is extracted 4 times with 100mL methyl tertiary butyl ether(MTBE)s respectively, the anhydrous MgSO of organic layer4It is dried overnight；
Filtrate is distilled after (2-3) filtering, obtains 137mmol, 10.7g fluoroacetic acid, yield 97%, purity is 99.6%；
(III) pure Fratol is prepared：Fluoroacetic acid will be obtained and be dissolved in second alcohol and water according to volume ratio 10:1 mixing being made into is molten
In liquid, saturation sodium hydroxide solution is then added dropwise, the material of NaOH in the saturation sodium hydroxide solution added
Measure as 1.05 times of the amount of fluoroacetic acid material in mixed solution, stir, pure Fratol is drying to obtain after filtering.With initial fluorine second
The amount of acid is calculated, and the yield of Fratol is 98%, and purity is 99.6%.
Embodiment 2
The preparation method of forensic science qualitative, quantitative Fratol, comprises the following steps：
(I) thick Fratol is prepared；
(1-1) 13.6mL (141mmol) ethyl fluoroacetate or methylfluoracetate is dissolved in 200mL methanol；
(1-2) adds 6.72g (168mmol) NaOH, and 20 hours are stirred at room temperature, white precipitate is slowly formed
Thing；
(1-3) and then decompression obtain thick Fratol, the thick Fratol solid of gained uses 30mL first respectively except solvent is to dry
Base tertbutyl ether is washed three times, removes organic impurities and the complete raw material of unreacted, is dried.
(II) fluoroacetic acid is prepared；
Thick Fratol is dissolved in the hydrochloric acid that HCl concentration is 3mol/L by (2-1), and adds NaCl to saturation；
(2-2) and then respectively with 100mL methyl tertiary butyl ether(MTBE)s extraction 4 times, merge organic layer, the anhydrous MgSO4 of organic layer
Dry, overnight；
Filtrate is distilled after (2-3) filtering, obtains 10.4g (133mmol) fluoroacetic acid, yield 95%, purity is 99.0%；
(III) pure Fratol is prepared：Fluoroacetic acid will be obtained and be dissolved in second alcohol and water according to volume ratio 10:1 mixing being made into is molten
In liquid, saturation sodium hydroxide solution is then added dropwise, the material of NaOH in the saturation sodium hydroxide solution added
Measure as 1.10 times of the amount of fluoroacetic acid material in mixed solution, stir, pure Fratol is drying to obtain after filtering.With initial fluorine second
The amount of acid is calculated, and the yield of Fratol is 97%, and purity is 99.0%.
Embodiment 3
The preparation method of forensic science qualitative, quantitative Fratol, comprises the following steps：
(I) thick Fratol is prepared；
(1-1) 13.6mL (141mmol) ethyl fluoroacetate or methylfluoracetate is dissolved in 200mL isopropanols and n-butanol
Mixed solution in, the volume ratio of isopropanol and n-butanol is 1:1；
(1-2) adds 6.72g (168mmol) NaOH, and 20 hours are stirred at room temperature, white precipitate is slowly formed
Thing；
(1-3) and then decompression obtain thick Fratol, the thick Fratol solid of gained uses 30mL first respectively except solvent is to dry
Base tertbutyl ether is washed three times, removes organic impurities and the complete raw material of unreacted, is dried.
(II) fluoroacetic acid is prepared；
Thick Fratol is dissolved in the hydrochloric acid that HCl concentration is 3mol/L by (2-1), and adds NaCl to saturation；
(2-2) and then respectively with 100mL methyl tertiary butyl ether(MTBE)s extraction 4 times, merge organic layer, the anhydrous MgSO4 of organic layer
Dry, overnight；
Filtrate is distilled after (2-3) filtering, obtains 10.5g (135mmol) fluoroacetic acid, yield 96%, purity is 99.0%；
(III) pure Fratol is prepared：Fluoroacetic acid will be obtained and be dissolved in second alcohol and water according to volume ratio 10:1 mixing being made into is molten
In liquid, saturation sodium hydroxide solution is then added dropwise, the material of NaOH in the saturation sodium hydroxide solution added
Measure as 1.10 times of the amount of fluoroacetic acid material in mixed solution, stir, pure Fratol is drying to obtain after filtering.With initial fluorine second
The amount of acid is calculated, and the yield of Fratol is 98%, and purity is 99.0%.
Embodiment 4
The preparation method of forensic science qualitative, quantitative Fratol, comprises the following steps：
(I) thick Fratol is prepared；
(1-1) 13.6mL (141mmol) ethyl fluoroacetate or methylfluoracetate is dissolved in the mixed of 200mL methanol and ethanol
Close in solution, the volume ratio of methanol and ethanol is 1:1；
(1-2) adds 6.72g (168mmol) NaOH, and 20 hours are stirred at room temperature, white precipitate is slowly formed
Thing；
(1-3) and then decompression obtain thick Fratol, the thick Fratol solid of gained uses 30mL first respectively except solvent is to dry
Base tertbutyl ether is washed three times, removes organic impurities and the complete raw material of unreacted, is dried.
(II) fluoroacetic acid is prepared；
Thick Fratol is dissolved in the hydrochloric acid that HCl concentration is 3mol/L by (2-1), and adds NaCl to saturation；
(2-2) and then respectively with 100mL methyl tertiary butyl ether(MTBE)s extraction 4 times, merge organic layer, the anhydrous MgSO4 of organic layer
Dry, overnight；
Filtrate is distilled after (2-3) filtering, obtains 10.5g (134mmol) fluoroacetic acid, yield 95%, purity is 99.0%；
(III) pure Fratol is prepared：Fluoroacetic acid will be obtained and be dissolved in second alcohol and water according to volume ratio 10:1 mixing being made into is molten
In liquid, saturation sodium hydroxide solution is then added dropwise, the material of NaOH in the saturation sodium hydroxide solution added
Measure as 1.10 times of the amount of fluoroacetic acid material in mixed solution, stir, pure Fratol is drying to obtain after filtering.With initial fluorine second
The amount of acid is calculated, and the yield of Fratol is 98%, and purity is 99.0%.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not pair
The restriction of embodiments of the present invention, for those of ordinary skill in the field, may be used also on the basis of the above description
To make other changes in different forms, all embodiments can not be exhaustive here, it is every to belong to this hair
Row of the obvious change or variation that bright technical scheme is extended out still in protection scope of the present invention.
Claims (9)
1. the preparation method of forensic science qualitative, quantitative Fratol, it is characterised in that comprise the following steps：(I) prepare thick
Fratol；(II) fluoroacetic acid is prepared；(III) pure Fratol is prepared：Fluoroacetic acid will be obtained and be dissolved in second alcohol and water according to volume ratio
10:In 1 mixed solution being made into, saturation sodium hydroxide solution is then added dropwise, in the saturation sodium hydroxide solution added
The amount of the material of NaOH is 1.05-1.10 times of the amount of fluoroacetic acid material in mixed solution, and stirring is drying to obtain after filtering
Pure Fratol.
2. the preparation method of forensic science qualitative, quantitative Fratol according to claim 1, it is characterised in that step
(I) comprise the following steps：(1-1) dissolves ethyl fluoroacetate or methylfluoracetate, and solute is made for ethyl fluoroacetate or fluorine second
The ethyl fluoroacetate solution or methylfluoracetate solution of sour methyl esters；(1-2) is to ethyl fluoroacetate solution or methylfluoracetate solution
Middle addition alkali, stirring；(1-3) is filtered, and filter residue is thick Fratol.
3. the preparation method of forensic science qualitative, quantitative Fratol according to claim 2, it is characterised in that in step
Suddenly in (1-1)：Ethyl fluoroacetate or methylfluoracetate are dissolved in alcohol, the volume ratio of solute and solvent is (2-3)：40.
4. the preparation method of forensic science qualitative, quantitative Fratol according to claim 3, it is characterised in that in step
Suddenly in (1-1)：Alcohol is any one or more in methanol, ethanol, isopropanol and n-butanol.
5. the preparation method of forensic science qualitative, quantitative Fratol according to claim 4, it is characterised in that in step
Suddenly in (1-2)：Alkali is added into ethyl fluoroacetate solution or methylfluoracetate solution, the addition of alkali is ethyl fluoroacetate or fluorine
1.05-1.5 times of the amount of the material of methyl acetate.
6. the preparation method of forensic science qualitative, quantitative Fratol according to claim 5, it is characterised in that in step
Suddenly in (1-2)：Alkali is NaOH or potassium hydroxide, is stirred 10-20 hours, generates white depositions, and vacuum distillation removes solvent
To dry, thick Fratol is obtained；In step (1-3), the thick Fratol solid of gained is washed with methyl tertiary butyl ether(MTBE), is removed organic
Impurity and the complete raw material of unreacted, are dried.
7. according to the preparation method of any described forensic science qualitative, quantitative Fratols of claim 1-6, its feature exists
In step (II) comprise the following steps：Thick Fratol is dissolved in acid solution by (2-1)；(2-2) uses Solvent Extract methods；
(2-3) is filtered to remove magnesium sulfate, and filtrate distillation is produced into fluoroacetic acid.
8. the preparation method of forensic science qualitative, quantitative Fratol according to claim 7, it is characterised in that in step
Suddenly in (2-1)：Acid solution is hydrochloric acid or sulfuric acid, and with corresponding sodium salt or sylvite saturation；Organic solvent is in step (2-2)
Organic layer is isolated after ether or methyl tertiary butyl ether(MTBE), extraction, and anhydrous magnesium sulfate is added in organic layer and is dried, overnight.
9. the preparation method of forensic science qualitative, quantitative Fratol according to claim 1, it is characterised in that including
Following steps：(I) thick Fratol is prepared；
141mmol, 13.6mL ethyl fluoroacetate or methylfluoracetate are dissolved in 240mL ethanol by (1-1)；
(1-2) adds 155mmol, 6.2g NaOH, and 12 hours are stirred at 50 c, generates white depositions；
(1-3) vacuum distillation obtains thick Fratol solid, the thick Fratol solid of gained uses 30mL first respectively except solvent is to dry
Base tertbutyl ether is washed three times, removes organic impurities and the complete raw material of unreacted, is dried；
(II) fluoroacetic acid is prepared；
Thick Fratol is added in the hydrochloric acid that HCl concentration is 3mol/L by (2-1), and regulation solution ph is 4, and adds NaCl
To saturation；
(2-2) is extracted 4 times with 100mL methyl tertiary butyl ether(MTBE)s respectively, merges organic phase, the anhydrous MgSO of organic layer4Dry, overnight；
Filtrate is distilled after (2-3) filtering, obtains 137mmol, 10.7g fluoroacetic acid.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013040790A1 (en) * | 2011-09-23 | 2013-03-28 | Merck Sharp & Dohme Corp. | Substituted pyrimidines |
| WO2013043624A1 (en) * | 2011-09-23 | 2013-03-28 | Merck Sharp & Dohme Corp. | Substituted pyrimidines |
| CN104945240A (en) * | 2015-06-01 | 2015-09-30 | 安徽华星化工有限公司 | Synthetic method of 2-methyl-4-chlorophenoxyacetic acid |
-
2017
- 2017-04-24 CN CN201710270296.2A patent/CN106946693A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013040790A1 (en) * | 2011-09-23 | 2013-03-28 | Merck Sharp & Dohme Corp. | Substituted pyrimidines |
| WO2013043624A1 (en) * | 2011-09-23 | 2013-03-28 | Merck Sharp & Dohme Corp. | Substituted pyrimidines |
| CN104945240A (en) * | 2015-06-01 | 2015-09-30 | 安徽华星化工有限公司 | Synthetic method of 2-methyl-4-chlorophenoxyacetic acid |
Non-Patent Citations (3)
| Title |
|---|
| CHRISTOPHER ALBLER, ET AL.: "Synthetic Routes towards Fluorine-Containing Amino Sugars: Synthesis of Fluorinated Analogues of Tomosamine and 4-Amino-4-deoxyarabinose", 《EUROPEAN JOURNAL OF ORGANIC CHEMISTRY》 * |
| 曾振芳 等: "苯氧乙酸合成工艺研究", 《广州化工》 * |
| 董建萍 等: "氯乙酸钠两种合成方法经济成本分析", 《现代商贸工业》 * |
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Application publication date: 20170714 |