CN102115431B - Synthesis method of 2, 2-ethoxyethanol - Google Patents
Synthesis method of 2, 2-ethoxyethanol Download PDFInfo
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Abstract
本发明涉及一种2，2-二乙氧基乙醇的合成方法，属于医药与化工技术领域。该方法是以式(I)化合物为原料通过和无机酸水解反应得到二氯乙酸；将制得的二氯乙酸与乙醇钠在无水乙醇中进行回流反应，反应结束后、冷却加入盐酸乙醇溶液，调pH、过滤、蒸馏，得到2，2-二乙氧基乙酸乙酯；再将步骤b制得的2，2-二乙氧基乙酸乙酯与KBH4和无机催化剂在无水乙醇中进行回流反应，制得2，2-二乙氧基乙醇。本发明的优点是原料易得、工艺过程简单、反应条件平稳、不需要在高压条件下进行反应、适合大规模工业化生产。溶剂乙醇可以回收套用，原子经济性好、成本低，所得产品收率高，产品质量达到98％以上。The invention relates to a synthesis method of 2,2-diethoxyethanol, which belongs to the technical field of medicine and chemical industry. The method uses the compound of formula (I) as a raw material to obtain dichloroacetic acid through hydrolysis reaction with inorganic acid; the prepared dichloroacetic acid and sodium ethylate are refluxed in absolute ethanol, and after the reaction is completed, the hydrochloric acid ethanol solution is added after cooling , adjust pH, filter, distill to obtain 2,2-diethoxy ethyl acetate; then the 2,2-diethoxy ethyl acetate prepared in step b is mixed with KBH 4 and inorganic catalyst in absolute ethanol Reflux reaction to produce 2,2-diethoxyethanol. The invention has the advantages of easy-to-obtain raw materials, simple process, stable reaction conditions, no need to react under high-pressure conditions, and is suitable for large-scale industrial production. The solvent ethanol can be recycled and used mechanically, the atom economy is good, the cost is low, the yield of the obtained product is high, and the product quality reaches more than 98%.
Description
Technical field
The present invention relates to a kind of synthetic method of medicine material, relate in particular to a kind of antiviral drug lamivudine raw material 2, the synthetic method of 2-diethoxyethanol belongs to medicine and chemical technology field.
Background technology
2,2-diethoxyethanol is the intermediate 1 of synthetic antiviral drug lamivudine, and the important source material of 3-oxygen thia ring-5-ketone compounds has important using value in organic synthesis and medicine synthetic field.
2,2-diethoxyethanol molecular formula is C
6H
14O
3, molecular weight is 134.17.Its structural formula is
In prior art 2,2-diethoxyethanol synthetic mainly contains following several scheme.Scheme one: as people such as William E.Parham at J.Am.Chem.Soc., 1955,77 (23), disclose in 6391-6393 with the phenylethyl alcohol raw material, with the synthetic phenylethyl alcohol sodium of sodium reaction, with the synthetic benzyl oxide of halo acetaldehyde contracting glycol reaction, at last the benzyl oxide reduction is obtained 2,2-diethoxyethanol again.Although adopt the method can synthesize 2,2-diethoxyethanol, the method synthesis technique is complicated, reaction conditions requires harsh, and cost is high.
Scheme two: as Chinese patent application (publication number: CN101624335A) relate to a kind of 2, the preparation method of 2 diethoxyethanols, the method is take the halo acetal as raw material, under the existence of alkali, carry out alkaline hydrolysis in water-water-miscible organic solvent mixed system, temperature of reaction is at 100 ℃～150 ℃, system pressure is under the condition of 0.14MPa～0.68MPa, reacted 2～72 hours, and made 2,2 diethoxyethanols.Alkali wherein is inorganic strong alkali (as potassium hydroxide, sodium hydroxide), and water-water-miscible organic solvent wherein can be water-soluble alcohol, ether, ketone or acid amides.Although having solved to a certain extent, the method synthesizes complex process in 2,2 diethoxyethanols, the problem that reaction cost is high take the halo acetal as raw material.But the method not only temperature of reaction is high, need to react under positive pressure, and conditional request is harsh, is unfavorable for large-scale industrial production; And the final product yield and purity lower.
Scheme three: relate to a kind ofly 2 as U.S. Patent application (publication number: US6518425 (B1)), the preparation method of 2-diethoxyethanol, the method are to be raw material with 2,2-diethoxy acetaldehyde, with NaHB
4Be catalyzer, through reduction reaction, make 2,2-diethoxyethanol.Although the method technical process is simple; Other side reaction easily occurs in the method, and the purity and the yield that finally obtain product are lower.
Summary of the invention
The present invention is directed to the existing defective of prior art, provide a kind of 2, the synthetic method of 2-diethoxyethanol; The method raw material is easy to get, and technological process is simple, and reaction conditions is gentle, and quality and the yield of the finished product are higher.
Above-mentioned purpose of the present invention is to be achieved by the following technical programs: a kind of 2, and the synthetic method of 2-diethoxyethanol, the method comprises the following steps:
A, take formula (I) compound as raw material by obtaining dichloro acetic acid with mineral acid hydrolysis reaction;
B, dichloro acetic acid and the sodium ethylate that makes in step a carried out back flow reaction in dehydrated alcohol, the cooling ethanol solution hydrochloride that adds after reaction finishes obtains 2,2-diethoxy acetic ether after transferring pH, filtration, distillation;
C, with step b make 2,2-diethoxy acetic ether and KBH
4Carry out back flow reaction with organic catalyst in dehydrated alcohol, reclaim dehydrated alcohol after reaction finishes and apply mechanically, then make 2,2-diethoxyethanol through aftertreatment;
R described in its Chinese style (I) is C
1～C
4Alkyl.
The present invention 2, and the concrete reaction equation of the synthetic method of 2-diethoxyethanol is as follows:
The present invention through hydrolysis reaction, makes dichloro acetic acid take formula (I) compound as starting raw material, then dichloro acetic acid and the sodium ethylate of gained reacted, and obtains 2,2-diethoxy acetic ether, then through hydrolysis, reduction, obtains 2,2-diethoxyethanol.The formula that the present invention not only adopts (I) compound, mineral acid, water are all to hold facile raw material in industrial production, and cheapness is conducive to suitability for industrialized production; And technological process is simple, does not need to react under condition of high voltage, and reaction conditions is gentle, and etoh solvent can recovery, has improved atom utilization, has also reduced greatly production cost.
Wherein the mass ratio of step a Chinese style (I) compound and mineral acid is 1: 0.02～1, and as preferably, mass ratio is 1: 0.05～0.3, and is further preferred, and quality is 1: 0.1.
The mass ratio of the dichloro acetic acid described in step b and sodium ethylate is 1: 8～15, be preferably 1: 8～and 10.The mass ratio of described dichloro acetic acid and acidic alcohol is 1: 1.2～2.5, be preferably 1: 1.2～and 2.0.As the ethoxylation agent, with the dichloro acetic acid reaction, generate 2,2-diethoxy acetic ether with sodium ethylate.In whole process, the sodium chloride salt of generation belongs to inorganic salt, substantially is insoluble to organic solvent, is easy to remove in last handling process.Be conducive to the recycling of solvent, operating process is simple, has also reduced greatly production cost.The mass concentration of described sodium ethylate is 5%～20%, is preferably 15%～18%.The mass concentration of described acidic alcohol is 20%～40%, is preferably 30%～38%.
In step c described in step c 2,2-diethoxy acetic ether and KBH
4Mass ratio be 1: 0.2～1, be preferably 1: 0.2～0.5.The mass ratio of 2,2-diethoxy acetic ether and organic catalyst is 1: 0.2～1, be preferably 1: 0.2～and 0.5.The detailed process of aftertreatment is to add organic solvent, and extraction, distillation obtain 2,2-diethoxyethanol; Described organic solvent is a kind of in benzene, toluene, ethyl acetate, diisopropyl ether, glycol dimethyl ether, ethylene glycol diethyl ether; As preferably, described organic solvent is a kind of in benzene, toluene or diisopropyl ether.
Above-mentioned 2, in the synthetic method of 2-diethoxyethanol, as preferably, the R in the formula described in step a (I) compound is methyl or ethyl.
Above-mentioned 2, in the synthetic method of 2-diethoxyethanol, the mineral acid described in step a is concentrated hydrochloric acid; The concentration of described concentrated hydrochloric acid is 30.0%～37.0%.
In step a, the temperature of hydrolysis reaction is 70 ℃～90 ℃, and hydrolysis time is 1～5 hour.Further preferred, the temperature of hydrolysis reaction is 80 ℃, and hydrolysis time is 2～3 hours.
Above-mentioned 2, in the synthetic method of 2-diethoxyethanol, in step b, the back flow reaction temperature is 50 ℃～80 ℃, and the time of back flow reaction is 2～8 hours.Further preferred, the back flow reaction temperature is 70 ℃～80 ℃, and reflux time is 4～6 hours.
Above-mentioned 2, in the synthetic method of 2-diethoxyethanol, be cooled to temperature after in step b, back flow reaction finishes and be 0-5 ℃ and drip ethanol solution hydrochloride; Further preferred, being cooled to temperature is 0 ℃ of dropping ethanol solution hydrochloride.Drip ethanol solution hydrochloride and can make reaction gentleer under cold condition, reduce the generation of side reaction, improve quality and the yield of product.
Above-mentioned 2, in the synthetic method of 2-diethoxyethanol, the organic catalyst described in step c is Li
2CO
3, LiCl, ZnCl
2, AlCl
3In a kind of.With Li
2CO
3, AlCl
3, ZnCl
2Deng as catalyzer, cost of material is cheap, convenient transportation, be easy to storage and production operation, is conducive to suitability for industrialized production.
Above-mentioned 2, in the synthetic method of 2-diethoxyethanol, in step c, the temperature of back flow reaction is 60 ℃～80 ℃, and the time of back flow reaction is 2～10 hours.Further preferred, the temperature of back flow reaction is 70 ℃～80 ℃, and the time of back flow reaction is 3～5 hours.
In sum, the present invention has the following advantages:
1, synthetic method Raw of the present invention is easy to get, and technological process is simple, and reaction conditions is steady, need to not react under condition of high voltage, and sufficient reacting, easily operation, can significantly reduce production costs, and is fit to large-scale industrial production.
2, in synthetic method of the present invention, etoh solvent can recovery, and Atom economy is good, and utilization ratio is high.
3, adopt 2 of synthetic method production of the present invention, 2-diethoxyethanol product yield is high, and quality product reaches more than 98%.
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in further detail; But the present invention is not limited to these embodiment.
Embodiment 1
Be that 36.5% hydrochloric acid 40g drops in the four-hole bottle of 1000ml with methyl dichloroacetate 400g, water 400ml and concentration, be warmed up to 80 ℃, hydrolysis reaction 2 hours, after reaction finished, air distillation steamed methyl dichloroacetate, water and methyl alcohol approximately after 80g, use underpressure distillation instead and control temperature less than 100 ℃, water in reaction system is steamed, steam complete after, slowly distillation heats up, first with the removal of before boiling, when rising to more than 120 ℃ to temperature, collect the fraction that steams, namely obtain dichloro acetic acid.
Dichloro acetic acid 75g, the 17.4% sodium ethylate 861g and the dehydrated alcohol 230g that make are dropped in the four-hole bottle of 1000ml, be warming up to 80 ℃ of backflows, reacted 4.5 hours, reaction is cooled to 0 ℃ after finishing, and begins to drip 37% ethanol solution hydrochloride 127.5g, in dripping, control temperature below 10 ℃, after dropwising, be warming up to 20 ℃ of reactions, after reaction finishes, be cooled to again 0 ℃, regulate pH value to 6.8 with sodium ethylate, in whole accent pH process, control temperature and be no more than 10 ℃, after mixing up, continue to stir 1 hour, remove by filter the sodium-chlor in system.The filtrate of gained is carried out underpressure distillation, namely obtain 2,2-diethoxy acetic ether.
At room temperature, with make 2,2-diethoxy acetic ether 100g, dehydrated alcohol 560g, 60gKBH
4And 60gLi
2CO
3Drop in the four-hole bottle of clean 1000ml, slowly be warming up to backflow, insulation reaction 4h is after reaction finishes, normal pressure steams ethanol to fluid not, and the ethanol of recovery is applied mechanically, and decompression steams residual ethanol evaporate to dryness more subsequently, then add water 100ml, be warming up to backflow, hydrolysis reaction 1 hour.After reaction finishes, then be cooled to proper temperature, decompression steams residual ethanol, be cooled at last room temperature, filter, collect filtrate, add salt of wormwood 100g to be stirred to dissolving in filtrate, add again the extraction of 600ml benzene, extract three times, collected organic layer carries out air distillation with the organic layer of gained, after reclaiming benzene, underpressure distillation is again steamed residual a small amount of benzene to the greatest extent, regathers temperature at 70 ℃, pressure is under the condition of 15mmHg, collect fraction, namely obtain 2,2-diethoxyethanol, yield reaches more than 80%, and quality product reaches more than 99%.
Embodiment 2
Be that 30.0% hydrochloric acid 120g drops in the four-hole bottle of 1000ml with methyl dichloroacetate 400g, water 400ml and concentration, be warmed up to 80 ℃, hydrolysis reaction 4 hours, after reaction finished, air distillation steamed methyl dichloroacetate, water and methyl alcohol approximately after 100g, use underpressure distillation instead and control temperature less than 100 ℃, water in reaction system is steamed, steam complete after, heat up, first with the removal of before boiling, when rising to more than 120 ℃ to temperature, collect the fraction that steams, namely obtain dichloro acetic acid.
Dichloro acetic acid 75g, the 15% sodium ethylate 600g and the dehydrated alcohol 250g that make are dropped in the four-hole bottle of 1000ml, be warming up to 76 ℃～80 ℃, reacted 6 hours, after reaction finishes, be cooled to 0 ℃, beginning to drip concentration is 40% ethanol solution hydrochloride 90g, controls temperature below 10 ℃, after dropwising, be warming up to 20 ℃ of reactions, after reaction finishes, then be cooled to 0 ℃, regulate pH value to 7.0 with sodium ethylate, in whole accent pH process, control temperature and be no more than 10 ℃, after mixing up, continue to stir 1 hour, remove by filter the sodium-chlor in system.The filtrate of gained is carried out underpressure distillation, namely obtain 2,2-diethoxy acetic ether.
At room temperature, with make 2,2-diethoxy acetic ether 100g, dehydrated alcohol 560g, 20gKBH
4And 100gLi
2CO
3Drop in the four-hole bottle of clean 1000ml, slowly be warming up to backflow, insulation reaction 6h is after reaction finishes, normal pressure steams ethanol to fluid not, and the ethanol of recovery is applied mechanically, and decompression steams residual ethanol evaporate to dryness more subsequently, then add water 100ml, be warming up to backflow, hydrolysis reaction 1 hour.after reaction finishes, be cooled to again proper temperature, decompression steams residual ethanol, be cooled at last room temperature, filter, collect filtrate, add salt of wormwood 100g to be stirred to dissolving in filtrate, add again the extraction of 600ml toluene, extract three times, each 600ml toluene of using, collect the organic layer of extraction used, the organic layer of gained is carried out air distillation, after reclaiming toluene, underpressure distillation again, residual a small amount of benzene is steamed to the greatest extent, control temperature at 70 ℃, pressure is under the condition of 15mmHg, collect fraction, namely obtain 2, the 2-diethoxyethanol, yield reaches more than 80%, quality product reaches more than 99%.
Embodiment 3
Be that 35.0% hydrochloric acid 50g drops in the four-hole bottle of 1000ml with ethyl dichloroacetate 400g, water 400ml and concentration, be warmed up to 80 ℃, hydrolysis reaction 3 hours, after reaction finished, air distillation steamed residual ethyl dichloroacetate, water and ethanol approximately after 110g, use underpressure distillation instead, control temperature less than 100 ℃, the water in reaction system is steamed, steam complete after, heat up and slowly distill, the removal of first before boiling is when rising to more than 120 ℃ to temperature, the fraction that collection steams namely obtains dichloro acetic acid.
Dichloro acetic acid 75g, the 18% sodium ethylate 870g and the dehydrated alcohol 230g that make are dropped in the four-hole bottle of 1000ml, be warming up to 70 ℃～75 ℃, reacted 6 hours, after reaction finishes, be cooled to 0 ℃, beginning to drip concentration is 30% ethanol solution hydrochloride 140g, controls temperature below 10 ℃, after dropwising, be warming up to 20 ℃ of reactions, after reaction finishes, then be cooled to 0 ℃, regulate pH value to 7.0 with sodium ethylate, in whole accent pH process, control temperature and be no more than 10 ℃, after mixing up, continue to stir 1 hour, remove by filter the sodium-chlor in system.The filtrate of gained is carried out underpressure distillation reclaim alcohol solvent, redistillation namely obtains 2,2-diethoxy acetic ether.
At room temperature, with make 2,2-diethoxy acetic ether 100g, dehydrated alcohol 560g, 50gKBH
4And 80gLi
2CO
3Drop in the four-hole bottle of clean 1000ml, slowly be warming up to backflow, insulation reaction 8h is after reaction finishes, normal pressure steams ethanol to fluid not, and the ethanol of recovery is applied mechanically, and decompression steams residual ethanol evaporate to dryness more subsequently, then add water 100ml, be warming up to backflow, hydrolysis reaction 1 hour.after reaction finishes, be cooled to again proper temperature, decompression steams residual ethanol, be cooled at last room temperature, filter, collect filtrate, add salt of wormwood 100g to be stirred to dissolving in filtrate, add again the extraction of 500ml diisopropyl ether, same method extraction three times, collected organic layer, the organic layer of gained is carried out air distillation, after reclaiming diisopropyl ether, underpressure distillation again, residual a small amount of diisopropyl ether is steamed to the greatest extent, regather temperature at 70 ℃, pressure is under the condition of 15mmHg, collect fraction, namely obtain 2, the 2-diethoxyethanol, yield reaches more than 80%, quality product reaches more than 99%.
Embodiment 4
Be that 33% hydrochloric acid 60g drops in the four-hole bottle of 1000ml with ethyl dichloroacetate 400g, water 400ml and concentration, be warmed up to 80 ℃, hydrolysis reaction 2 hours, after reaction finished, air distillation steamed ethyl dichloroacetate, water and ethanol approximately after 90g, use underpressure distillation instead and control temperature less than 100, water in reaction system is steamed, steam complete after, heat up, boil before boiling off, when rising to more than 120 ℃ to temperature, begin to collect the fraction that steams, namely obtain dichloro acetic acid.
Dichloro acetic acid 75g, the 20% sodium ethylate 900g and the dehydrated alcohol 250g that make are dropped in the four-hole bottle of 1500ml, be warming up to backflow, reacted 4 hours, reaction is cooled to 0 ℃ after finishing, and beginning to drip concentration is 40% ethanol solution hydrochloride 113g, after dropwising, be warming up to 20 ℃ of reactions, after reaction finishes, be cooled to again 0 ℃, regulate pH value to 6.8 with sodium ethylate, in whole accent pH process, control temperature and be no more than 10C, after mixing up, continue to stir 1 hour, remove by filter the sodium-chlor in system.The filtrate of gained is carried out decompression recycling ethanol, and redistillation namely obtains 2,2-diethoxy acetic ether.
At room temperature, with make 2,2-diethoxy acetic ether 100g, dehydrated alcohol 600g, 50gKBH
4With 50g ZnCl
2Drop in the four-hole bottle of clean 1000ml, slowly be warming up to backflow, insulation reaction 8h is after reaction finishes, normal pressure steams ethanol to fluid not, and the ethanol of recovery is applied mechanically, and decompression steams residual ethanol evaporate to dryness more subsequently, then add water 110ml, be warming up to backflow, hydrolysis reaction 1 hour.after reaction finishes, be cooled to again proper temperature, decompression steams residual ethanol, be cooled at last room temperature, filter, collect filtrate, add salt of wormwood 100g to be stirred to dissolving in filtrate, add again the 500ml ethyl acetate extraction, collected organic layer, same method extraction three times, the organic layer that three extractions are collected merges, carry out air distillation, after reclaiming ethyl acetate, underpressure distillation again, residual a small amount of benzene is steamed to the greatest extent, regather temperature at 70 ℃, pressure is under the condition of 15mmHg, collect fraction, namely obtain 2, the 2-diethoxyethanol, yield reaches more than 80%, quality product reaches more than 99%.
Embodiment 5
At room temperature, will by embodiment 1 method make 2,2-diethoxy acetic ether 100g, reclaim ethanol 600g, 50gKBH
4Drop in the four-hole bottle of clean 1000ml with 30g LiCl, slowly be warming up to backflow, insulation reaction 8h, after reaction finished, normal pressure steamed ethanol to fluid not, and the ethanol of recovery is applied mechanically, decompression steams residual ethanol evaporate to dryness more subsequently, then add water 110ml, be warming up to backflow, hydrolysis reaction 1 hour.after reaction finishes, be cooled to again proper temperature, decompression steams residual ethanol, be cooled at last room temperature, filter, collect filtrate, add salt of wormwood 100g to be stirred to dissolving in filtrate, add again the extraction of 500ml ethylene glycol diethyl ether, collected organic layer, same method extraction three times, the organic layer that three extractions are collected merges, carry out air distillation, after reclaiming ethylene glycol diethyl ether, underpressure distillation again, residual a small amount of ethylene glycol diethyl ether is steamed to the greatest extent, regather temperature at 70 ℃, pressure is under the condition of 15mmHg, collect fraction, namely obtain 2, the 2-diethoxyethanol, yield reaches more than 80%, content reaches more than 99%.
Embodiment 6
At room temperature, will make by the method for embodiment 12,2-diethoxy acetic ether 100g, reclaim ethanol 600g, 50gKBH
4With 30g AlCl
3Drop in the four-hole bottle of clean 1000ml, slowly be warming up to backflow, insulation reaction 5h is after reaction finishes, normal pressure steams ethanol to fluid not, and the ethanol of recovery is applied mechanically, and decompression steams residual ethanol evaporate to dryness more subsequently, then add water 110ml, be warming up to backflow, hydrolysis reaction 1 hour.after reaction finishes, be cooled to again proper temperature, decompression steams residual ethanol, be cooled at last room temperature, filter, collect filtrate, add salt of wormwood 100g to be stirred to dissolving in filtrate, add again the extraction of 500ml benzene, collected organic layer, same method extraction three times, the organic layer that three extractions are collected merges, carry out air distillation, after reclaiming benzene, underpressure distillation again, residual a small amount of benzene is steamed to the greatest extent, regather temperature at 70 ℃, pressure is under the condition of 15mmHg, collect fraction, namely obtain 2, the 2-diethoxyethanol, yield reaches more than 80%, content reaches more than 99%.
Specific embodiment described in the present invention is only to the explanation for example of the present invention's spirit.Those skilled in the art can make various modifications or replenish or adopt similar mode to substitute described specific embodiment, but can't depart from spirit of the present invention or surmount the defined scope of appended claims.
Although the present invention has been made a detailed description and has quoted as proof some specific embodiments, to those skilled in the art, only otherwise it is obvious leaving that the spirit and scope of the present invention can make various changes or revise.
Claims (7)
1. one kind 2, the synthetic method of 2-diethoxyethanol, the method comprises the following steps:
A, take the formula I compound as raw material by obtaining dichloro acetic acid with mineral acid hydrolysis reaction;
B, dichloro acetic acid and the sodium ethylate that makes in step a carried out back flow reaction in dehydrated alcohol, the cooling ethanol solution hydrochloride that adds after reaction finishes obtains 2,2-diethoxy acetic ether after transferring pH, filtration, distillation;
C, with step b make 2,2-diethoxy acetic ether and KBH
4Carry out back flow reaction with organic catalyst in dehydrated alcohol, reclaim dehydrated alcohol after reaction finishes and apply mechanically, then make 2,2-diethoxyethanol through aftertreatment; And described organic catalyst is Li
2CO
3, LiCl, ZnCl
2, AlCl
3In a kind of;
Wherein the R described in formula I is C
1～C
4Alkyl.
2. according to claim 12, the synthetic method of 2-diethoxyethanol is characterized in that: the R in the formula I compound described in step a is methyl or ethyl.
3. described 2 according to claim 1 and 2, the synthetic method of 2-diethoxyethanol is characterized in that: the mineral acid described in step a is concentrated hydrochloric acid.
4. according to claim 32, the synthetic method of 2-diethoxyethanol is characterized in that: in step a, the temperature of hydrolysis reaction is 70 ℃～90 ℃, and hydrolysis time is 1～5 hour.
5. according to claim 12, the synthetic method of 2-diethoxyethanol is characterized in that: in step b, the back flow reaction temperature is 50 ℃～80 ℃, and the time of back flow reaction is 2～8 hours.
6. according to claim 1 or 52, the synthetic method of 2-diethoxyethanol is characterized in that: be cooled to temperature after in step b, back flow reaction finishes and be 0-5 ℃ and drip ethanol solution hydrochloride.
7. according to claim 12, the synthetic method of 2-diethoxyethanol is characterized in that: in step c, the temperature of back flow reaction is 60 ℃～80 ℃, and the time of back flow reaction is 2～10 hours.
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