CN107814778A - A kind of α acetyl group gamma butyrolactone continuous stream microchannel plate answers production technology - Google Patents
A kind of α acetyl group gamma butyrolactone continuous stream microchannel plate answers production technology Download PDFInfo
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- CN107814778A CN107814778A CN201711043439.2A CN201711043439A CN107814778A CN 107814778 A CN107814778 A CN 107814778A CN 201711043439 A CN201711043439 A CN 201711043439A CN 107814778 A CN107814778 A CN 107814778A
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- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/26—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member
- C07D307/30—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
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- C07D307/33—Oxygen atoms in position 2, the oxygen atom being in its keto or unsubstituted enol form
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Abstract
The invention discloses a kind of α acetyl group gamma butyrolactone continuous stream microchannel plate to answer production technology; using acetoacetic ester and oxirane as raw material; added in alcohols solvent under alkali metal component effect; reaction temperature is 10 80 DEG C; the residence time of reaction is 5 hours 1 second; reaction pressure is 0.1 2Mpa, reacts generation aceto butyrolactone through continuous stream micro passage reaction continuous condensating, obtains condensation reaction solution；Oxirane is 1 1.1 to the mol ratio of acetoacetic ester, and alkali metal component is 0.9 1.1 to the mol ratio of acetoacetic ester, and alcoholic solvent is 14 to the mass ratio of acetoacetic ester.The condensation reaction solution is neutralized with acid solution, control ph be 58, after neutralization under 10 50kPa pressure 40 80 DEG C of continuous evaporations；20 40 DEG C are cooled to after evaporation with 0.1 1:The organic solvent extracting and demixing of 1 mass ratio, the organic layer being obtained by extraction passes through desolventizing tower desolvation, then rectifying obtains product α acetyl gamma butyrolactones under 0.1 1kpa pressure.The method high income of the present invention, comprehensive production cost are less than butyrolactone method.Simultaneously because using technique is continuously synthesizing to, security also greatly improves.
Description
Technical field
The present invention relates to belong to chemical industry synthesis field, and in particular to the production method of α-acetyl group-gamma-butyrolacton.
Background technology
α-acetyl group-gamma-butyrolacton
The entitled 2-Acetylbutyrolactone of English, abbreviation aceto butyrolactone, english abbreviation ABL.
Molecular formula：C6H8O3
Outward appearance：Colourless transparent liquid.
Dissolubility：Solubility is 20% in water.
Molecular weight：128.13
Boiling point：253℃
Density：1.191g/cm3
Flash-point：128℃
Relative density:1.17
Purposes：
α-acetyl-gamma-butyrolacton (ABL) is the raw material (being mainly used in synthesizing vitamin B1) and leaf for preparing vitamins
The main intermediate of chlorins, it can be additionally used in medical industry manufacture antianginal drug and prolong pained medicine of Denging.Especially with dimension
Raw plain B1, to prolong pained, chloroquine, bactericide prothioconazoles, anticonvulsant drug Clomethiazole Hydrochloride, antischizophrenic drugs of Risperidone phonetic
The continuous developing of pyridine and special medical high polymer material at home and abroad in the market, increases ABL demand, before market year by year
Scape is boundless.
Prior art synthesis technique：
Its industrial production of α-acetyl group-gamma-butyrolacton mainly has two methods：
First, carry out the method for condensation reaction under sodium alkoxide effect with ethyl acetate in atent solvent by gamma-butyrolacton.
The technique is the domestic method that industrialized production generally uses at present.But the production technology makees solvent using toluene, and in gold
Belong to the mixture that ethyl acetate and gamma-butyrolacton are added dropwise under sodium molten condition, in reaction initiating stage, generation is largely easily gasified
Acetic acid esters and reaction generation by-product ethanol, hydrogen, easily occur slug, burning, even explode etc. accident.
Second, acetoacetic ester is condensed closed loop again in methanol or ethanol with oxirane with sodium alkoxide or sodium hydroxide effect
Method, but the method using batch process produce, the reaction time length, side reaction is more, and yield is not high, with former approach than produce
Cost is high.
The content of the invention
Therefore, the technical problem to be solved in the present invention is, there is provided a kind of technique is simple, the high α-acetyl of reaction efficiency
Base-gamma-butyrolacton continuous stream microchannel plate answers production technology.
The technical scheme is that a kind of α-acetyl group-gamma-butyrolacton continuous stream microchannel plate answers production technology, with
Acetoacetic ester and oxirane are raw material, are added in alcohols solvent under alkali metal component effect, reaction temperature 10-80
DEG C, the residence time of reaction is -5 hours 1 second, reaction pressure 0.1-2Mpa, through continuous stream micro passage reaction continuous condensating
Reaction generation aceto butyrolactone, obtains condensation reaction solution；Oxirane is 1-1.1 to the mol ratio of acetoacetic ester, alkali metal
Composition is 0.9-1.1 to the mol ratio of acetoacetic ester, and alcoholic solvent is 1-4 to the mass ratio of acetoacetic ester.
The condensation reaction solution that above-mentioned condensation reaction obtains is neutralized with acid solution, control ph 5-8, in 10- after neutralization
40-80 DEG C of continuous evaporation under 50kPa pressure；20-40 DEG C is cooled to after evaporation with 0.1-1:The organic solvent extraction point of 1 mass ratio
Layer, the organic layer being obtained by extraction passes through desolventizing tower desolvation, then rectifying obtains product α-acetyl-under 0.1-1kpa pressure
Gamma-butyrolacton.
Preferably, the residence time of reaction is -5 hours 0.5 hour.
Production technology is answered according to a kind of α-acetyl group-gamma-butyrolacton continuous stream microchannel plate of the present invention, it is preferred that
The acetoacetic ester is Acetacetic acid alkyl ester, selected from methyl acetoacetate, ethyl acetoacetate, butyl-acetoacetate, second
One kind in the ethyl acetoacetic acid tert-butyl ester.
Further, the acetoacetic ester is methyl acetoacetate.
Production technology is answered according to a kind of α-acetyl group-gamma-butyrolacton continuous stream microchannel plate of the present invention, it is preferred that
The one kind of the alcohols solvent in methanol, ethanol, propyl alcohol, butanol, ethylene glycol.
Production technology is answered according to a kind of α-acetyl group-gamma-butyrolacton continuous stream microchannel plate of the present invention, it is preferred that
The alkali metal component is selected from alkali metal hydroxide or alkali alcoholate.
Further, the alkali metal is selected from sodium and potassium.
Further, alkali metal component is preferably sodium hydroxide or sodium methoxide.I.e. alkali metal hydroxide is more preferably hydrogen
Sodium oxide molybdena, alkali alcoholate are more preferably sodium methoxide.
Production technology is answered according to a kind of α-acetyl group-gamma-butyrolacton continuous stream microchannel plate of the present invention, it is preferred that
The described organic solvent of extraction is aromatic hydrocarbon solvent, one kind in esters solvent, halogen class solvent.
Production technology is answered according to a kind of α-acetyl group-gamma-butyrolacton continuous stream microchannel plate of the present invention, it is preferred that
The acid solution is hydrochloric acid solution, dilution heat of sulfuric acid, phosphoric acid,diluted, the one or more of spirit of vinegar.It is further preferred that dilute sulfuric acid is molten
Liquid is 20-65% sulfuric acid solutions.
Production technology is answered according to a kind of α-acetyl group-gamma-butyrolacton continuous stream microchannel plate of the present invention, it is preferred that
After the continuous evaporation, alcohol reuse after dehydration is reclaimed；Recovered solvent is recyclable to be applied to extraction, the second obtained in rectifying
Ethyl sodio acetoacetic ester Recovery and recycle is used in condensation reaction.
Present invention is generally directed to original production technology acetoacetic ester and oxirane, alkali metal component is made in alcoholic solvent
Grown with lower using batch process condensation reaction time, the problem of side reaction is more, and yield is not high, have developed new continuity method production work
Skill.
The beneficial effects of the invention are as follows：
Continuous stream high flux microchannel reaction system is applied to second by the present invention for the technology and reaction equipment of core
In the condensation reaction of ethyl sodio acetoacetic ester and oxirane, process conditions are enhanced, improve reaction efficiency, realize the company of the product
Continuous, safe efficient, steady production, product purity and quality significantly improve, compared with traditional batch technique, reaction process process
Controllability greatly promote, reaction unit efficiency significantly increases, and continuous operation and the reaction zone inventory being greatly reduced made
The danger of journey significantly reduces, and the production capacity of unit volume process units is multiplied, in augmentation of heat transfer, mass transfer, environmental protection and peace
There is reliable guarantee in all directions, by process intensification, accurate temperature controlling, the reaction time is short and reduces the technologies such as reaction liquid holdup
Means drastically reduce the area the generation of side reaction, so as to avoid the shortcomings that oxirane low boiling point is inflammable and explosive.This technique makes
Raw material acetoacetic ester conversion per pass reaches more than 84%, ABL once through yields and reaches more than 68%, total recovery reach 80% with
On.Methanol, toluene and unreacted acetoacetic ester are recyclable to be applied mechanically, and this process recovery ratio is high, and comprehensive production cost is less than in fourth
Ester process.Simultaneously because using technique is continuously synthesizing to, security also greatly improves.The project overall technology has filled up domestic sky
In vain, reach advanced world standards.
Using batch process, acetoacetic ester is condensed with oxirane in alcoholic solvent under alkali metal component effect
The problems such as there is reaction time length in reaction, side reaction is more, and yield is not high, it is anti-through Novel connection afterflow micro passage reaction continuous condensating
Aceto butyrolactone should be generated, the reaction time is short, safe, stable operation is reliable, yield significantly improves.
Embodiment
Embodiment 1：
A kind of α-acetyl group-gamma-butyrolacton continuous stream microchannel plate answers production technology, comprises the following steps：
Solid sodium hydroxide addition methanol is configured to 20% methanol solution with 400g/h, methyl acetoacetate 232g/
H, oxirane 92g/h (n methyl acetoacetates：N oxirane：N sodium hydroxide=1:1.05:1) while with pump it is pumped into micro- logical
In road reactor, in 50 DEG C, 0.5Mpa, residence time 1 it is small react at present, the reaction solution of outlet is by 30% sulfuric acid with 360g/h's
Speed is added thereto, and pH to 5.5 is adjusted, into evaporator continuous evaporation methanol, operating pressure 20kpa, temperature 70 C.Steam
Reuse after methanol dehydration, kettle liquid are cooled to 35 DEG C and deliver to extraction column overhead, the first with entering extraction tower bottom with 150g/h simultaneously
Benzene carries out counter-current extraction, and the organic phase of extraction enters desolventizing tower, operating pressure 15kpa, the toluene reuse steamed to extraction.It is de-
Except the kettle liquid after toluene enters vacuum rectification tower, operating pressure 0.65kpa, obtained methyl acetoacetate 36g/h is back to contracting
Close reaction, obtained product α-acetyl group-gamma-butyrolacton 175g/h, content 99.3% (GC), once through yield 68.4%, conversion
Rate 84.5%, total recovery 80.9%.
Embodiment 2：
Solid sodium hydroxide addition methanol is configured to 20% methanol solution with 440g/h, methyl acetoacetate 232g/
H, oxirane 96g/h (n methyl acetoacetates：N oxirane：N sodium hydroxide=1:1.1:1.1) while with pump it is pumped into micro- logical
In road reactor, in 50 DEG C, 0.5Mpa, residence time 1 it is small react at present, the reaction solution of outlet is by 30% sulfuric acid with 393g/h's
Speed is added thereto, and pH to 5.5 is adjusted, into evaporator continuous evaporation methanol, operating pressure 20kpa, temperature 70 C.Steam
Reuse after methanol dehydration, kettle liquid are cooled to 35 DEG C and deliver to extraction column overhead, the first with entering extraction tower bottom with 150g/h simultaneously
Benzene carries out counter-current extraction, and the organic phase of extraction enters desolventizing tower, operating pressure 15kpa, the toluene reuse steamed to extraction.It is de-
Except the kettle liquid after toluene enters vacuum rectification tower, operating pressure 0.65kpa, obtained methyl acetoacetate 35g/h is back to contracting
Close reaction, obtained product α-acetyl group-gamma-butyrolacton 174g/h, content 99.3% (GC), once through yield 68.0%, conversion
Rate 84.9%, total recovery 80.0%.
Embodiment 3：
Solid sodium hydroxide addition methanol is configured to 20% methanol solution with 360g/h, methyl acetoacetate 232g/
H, oxirane 88g/h (n methyl acetoacetates：N oxirane：N sodium hydroxide=1:1:0.9) while with pump it is pumped into microchannel
In reactor, in 50 DEG C, 0.5Mpa, residence time 1 it is small react at present, the reaction solution of outlet is by 30% sulfuric acid with 328g/h speed
Degree is added thereto, and pH to 5.5 is adjusted, into evaporator continuous evaporation methanol, operating pressure 20kpa, temperature 70 C.The first steamed
Reuse after dehydration of alcohols, kettle liquid are cooled to 35 DEG C and deliver to extraction column overhead, the toluene with entering extraction tower bottom with 150g/h simultaneously
Counter-current extraction is carried out, the organic phase of extraction enters desolventizing tower, operating pressure 15kpa, the toluene reuse steamed to extraction.Removing
Kettle liquid after toluene enters vacuum rectification tower, operating pressure 0.65kpa, and obtained methyl acetoacetate 37g/h is back to condensation
Reaction, obtained product α-acetyl group-gamma-butyrolacton 174g/h, content 99.2% (GC), once through yield 68.0%, conversion ratio
84.1%, total recovery 80.9%.
Embodiment 4：
Solid sodium hydroxide addition methanol is configured to 20% methanol solution with 400g/h, methyl acetoacetate 232g/
H, oxirane 92g/h (n methyl acetoacetates：N oxirane：N sodium hydroxide=1:1.05:1) while with pump it is pumped into micro- logical
In road reactor, in 40 DEG C, 0.4Mpa, residence time 2 it is small react at present, the reaction solution of outlet is by 30% sulfuric acid with 360g/h's
Speed is added thereto, and pH to 5.5 is adjusted, into evaporator continuous evaporation methanol, operating pressure 20kpa, temperature 70 C.Steam
Reuse after methanol dehydration, kettle liquid are cooled to 35 DEG C and deliver to extraction column overhead, the first with entering extraction tower bottom with 150g/h simultaneously
Benzene carries out counter-current extraction, and the organic phase of extraction enters desolventizing tower, operating pressure 15kpa, the toluene reuse steamed to extraction.It is de-
Except the kettle liquid after toluene enters vacuum rectification tower, operating pressure 0.65kpa, obtained methyl acetoacetate 36g/h is back to contracting
Close reaction, obtained product α-acetyl group-gamma-butyrolacton 175g/h, content 99.3% (GC), once through yield 68.4%, conversion
Rate 84.5%, total recovery 80.9%.
Embodiment 5：
Solid sodium hydroxide addition methanol is configured to 20% methanol solution with 400g/h, methyl acetoacetate 232g/
H, oxirane 92g/h (n methyl acetoacetates：N oxirane：N sodium hydroxide=1:1.05:1) while with pump it is pumped into micro- logical
In road reactor, in 40 DEG C, 0.4Mpa, residence time 2 it is small react at present, the reaction solution of outlet is by 40% sulfuric acid with 270g/h's
Speed is added thereto, and pH to 5.5 is adjusted, into evaporator continuous evaporation methanol, operating pressure 20kpa, temperature 70 C.Steam
Reuse after methanol dehydration, kettle liquid are cooled to 35 DEG C and deliver to extraction column overhead, the first with entering extraction tower bottom with 150g/h simultaneously
Benzene carries out counter-current extraction, and the organic phase of extraction enters desolventizing tower, operating pressure 15kpa, the toluene reuse steamed to extraction.It is de-
Except the kettle liquid after toluene enters vacuum rectification tower, operating pressure 0.65kpa, obtained methyl acetoacetate 36g/h is back to contracting
Close reaction, obtained product α-acetyl group-gamma-butyrolacton 175g/h, content 99.3% (GC), once through yield 68.4%, conversion
Rate 84.5%, total recovery 80.9%.
Embodiment 6：
Sodium methoxide addition methanol is configured to 27% methanol solution with 400g/h, methyl acetoacetate 232g/h, epoxy
Ethane 92g/h (n methyl acetoacetates：N oxirane：N sodium methoxide=1:1.05:1) while with pump it is pumped into micro passage reaction
In, in 50 DEG C, 0.5Mpa, residence time 1 it is small react at present, the reaction solution of outlet adds 30% sulfuric acid with 360g/h speed
Wherein, pH to 5.5 is adjusted, into evaporator continuous evaporation methanol, operating pressure 20kpa, temperature 70 C.The methanol dehydration steamed
Reuse afterwards, kettle liquid are cooled to 35 DEG C and deliver to extraction column overhead, and the toluene progress that tower bottom is extracted with entering with 150g/h simultaneously is inverse
Stream extraction, the organic phase of extraction enter desolventizing tower, operating pressure 15kpa, the toluene reuse steamed to extraction.After removing toluene
Kettle liquid enter vacuum rectification tower, operating pressure 0.65kpa, obtained methyl acetoacetate 36g/h is back to condensation reaction, obtained
Product α-acetyl group-gamma-butyrolacton the 175g/h arrived, content 99.3% (GC), once through yield 68.4%, conversion ratio 84.5%,
Total recovery 80.9%.
Embodiment 7：
Solid sodium hydroxide addition ethanol is configured to 20% ethanol solution with 400g/h, ethyl acetoacetate 260g/
H, oxirane 92g/h (n ethyl acetoacetates：N oxirane：N sodium hydroxide=1:1.05:1) while with pump it is pumped into micro- logical
In road reactor, in 50 DEG C, 0.5Mpa, residence time 1 it is small react at present, the reaction solution of outlet is by 30% sulfuric acid with 360g/h's
Speed is added thereto, and pH to 5.5 is adjusted, into evaporator continuous evaporation ethanol, operating pressure 20kpa, 75 DEG C of temperature.Steam
Reuse after ethanol dehydration, kettle liquid are cooled to 35 DEG C and deliver to extraction column overhead, the first with entering extraction tower bottom with 150g/h simultaneously
Benzene carries out counter-current extraction, and the organic phase of extraction enters desolventizing tower, operating pressure 15kpa, the toluene reuse steamed to extraction.It is de-
Except the kettle liquid after toluene enters vacuum rectification tower, operating pressure 0.65kpa, obtained ethyl acetoacetate 41g/h is back to contracting
Close reaction, obtained product α-acetyl group-gamma-butyrolacton 174g/h, content 99.3% (GC), once through yield 68.0%, conversion
Rate 84.2%, total recovery 80.7%.
Comparative example 1：
Solid sodium hydroxide addition methanol is configured to 20% methanol solution with 480g/h, methyl acetoacetate 232g/
H, oxirane 106g/h (n methyl acetoacetates：N oxirane：N sodium hydroxide=1:1.2:1.2) while with pump it is pumped into micro-
In channel reactor, in 50 DEG C, 0.5Mpa, residence time 1 it is small react at present, the reaction solution of outlet is by 30% sulfuric acid with 426g/h
Speed be added thereto, adjust pH to 5.5, into evaporator continuous evaporation methanol, operating pressure 20kpa, temperature 70 C.Steam
Methanol dehydration after reuse, kettle liquid is cooled to 35 DEG C and delivers to extraction column overhead, with entering extraction tower bottom simultaneously with 150g/h
Toluene carries out counter-current extraction, and the organic phase of extraction enters desolventizing tower, operating pressure 15kpa, the toluene reuse steamed to extraction.
Kettle liquid after removing toluene enters vacuum rectification tower, operating pressure 0.65kpa, and obtained methyl acetoacetate 26g/h is back to
Condensation reaction, obtained product α-acetyl group-gamma-butyrolacton 146g/h, content 99.3% (GC), once through yield 57.0%, turn
Rate 88.8%, total recovery 64.2%.
When the equivalent of oxirane and sodium hydroxide increases to 1.2, reaction speed increase, but the α-acetyl group-γ generated-
The formation speed that the decomposition rate increase of butyrolactone is greater than main reaction increases, under the yield for causing α-acetyl group-gamma-butyrolacton
Drop.
The present invention is disclosed with preferred embodiment above, so it is not intended to limiting the invention, all to use equivalent substitution
Or the technical scheme that equivalent transformation mode is obtained, it is within the scope of the present invention.
Claims (9)
1. a kind of α-acetyl group-gamma-butyrolacton continuous stream microchannel plate answers production technology, it is characterised in that：With acetoacetic ester
It is raw material with oxirane, is added in alcohols solvent under alkali metal component effect, reaction temperature is 10-80 DEG C, and reaction stops
It is -5 hours 1 second, reaction pressure 0.1-2Mpa to stay the time, reacts generation acetyl through continuous stream micro passage reaction continuous condensating
Butyrolactone, obtain condensation reaction solution；Oxirane is 1-1.1 to the mol ratio of acetoacetic ester, and alkali metal component is to acetyl second
The mol ratio of acid esters is 0.9-1.1, and alcoholic solvent is 1-4 to the mass ratio of acetoacetic ester.
The condensation reaction solution is neutralized with acid solution, control ph 5-8, after neutralization under 10-50kPa pressure 40-80 DEG C of company
Continuous evaporation；20-40 DEG C is cooled to after evaporation with 0.1-1:The organic solvent extracting and demixing of 1 mass ratio, the organic layer being obtained by extraction
By desolventizing tower desolvation, then rectifying obtains product α-acetyl-gamma-butyrolacton under 0.1-1kpa pressure.
2. a kind of α-acetyl group-gamma-butyrolacton continuous stream microchannel plate according to claim 1 answers production technology, it is special
Sign is：The acetoacetic ester is Acetacetic acid alkyl ester, selected from methyl acetoacetate, ethyl acetoacetate, acetoacetate
One kind in butyl ester, tert-butyl acetoacetate.
3. a kind of α-acetyl group-gamma-butyrolacton continuous stream microchannel plate according to claim 2 answers production technology, it is special
Sign is：The acetoacetic ester is methyl acetoacetate.
4. a kind of α-acetyl group-gamma-butyrolacton continuous stream microchannel plate according to claim 1 answers production technology, it is special
Sign is：The one kind of the alcohols solvent in methanol, ethanol, propyl alcohol, butanol, ethylene glycol.
5. a kind of α-acetyl group-gamma-butyrolacton continuous stream microchannel plate according to claim 1 answers production technology, it is special
Sign is：Alkali metal component is selected from alkali metal hydroxide or alkali alcoholate.
6. a kind of α-acetyl group-gamma-butyrolacton continuous stream microchannel plate according to claim 5 answers production technology, it is special
Sign is：The alkali metal is selected from sodium and potassium.
7. a kind of α-acetyl group-gamma-butyrolacton continuous stream microchannel plate according to claim 1 answers production technology, it is special
Sign is：The described organic solvent of extraction is aromatic hydrocarbon solvent, one kind in esters solvent, halogen class solvent.
8. a kind of α-acetyl group-gamma-butyrolacton continuous stream microchannel plate according to claim 1 answers production technology, it is special
Sign is：The acid solution is hydrochloric acid solution, dilution heat of sulfuric acid, phosphoric acid,diluted, the one or more of spirit of vinegar.
9. a kind of α-acetyl group-gamma-butyrolacton continuous stream microchannel plate according to claim 1 answers production technology, it is special
Sign is：After the continuous evaporation, alcohol reuse after dehydration is reclaimed；Recovered solvent is recyclable to be applied to extraction, in rectifying
Obtained acetoacetic ester Recovery and recycle is used in condensation reaction.
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| US11618727B2 (en) | 2021-02-26 | 2023-04-04 | Fudan University | Method for preparing 3-chloro-4-oxopentyl acetate using fully continuous-flow micro-reaction system |
| CN117720487A (en) * | 2023-12-16 | 2024-03-19 | 深圳智微通科技有限公司 | Method for continuously synthesizing alpha-acetyl-gamma-butyrolactone |
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| CN111018810A (en) * | 2019-12-13 | 2020-04-17 | 浙江联盛化学股份有限公司 | Device and method for continuously producing α -acetyl-gamma-butyrolactone |
| CN111018810B (en) * | 2019-12-13 | 2021-09-14 | 浙江联盛化学股份有限公司 | Device and method for continuously producing alpha-acetyl-gamma-butyrolactone |
| US11618727B2 (en) | 2021-02-26 | 2023-04-04 | Fudan University | Method for preparing 3-chloro-4-oxopentyl acetate using fully continuous-flow micro-reaction system |
| CN114044763A (en) * | 2022-01-13 | 2022-02-15 | 山东国邦药业有限公司 | Method for synthesizing gamma-butyrolactone |
| CN117720487A (en) * | 2023-12-16 | 2024-03-19 | 深圳智微通科技有限公司 | Method for continuously synthesizing alpha-acetyl-gamma-butyrolactone |
| CN117720487B (en) * | 2023-12-16 | 2024-08-06 | 深圳智微通科技有限公司 | Method for continuously synthesizing alpha-acetyl-gamma-butyrolactone |
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