CN105837440B - A kind of preparation process of the chloro- 2- acetyl group methoxy propane of 1,3- bis- - Google Patents
A kind of preparation process of the chloro- 2- acetyl group methoxy propane of 1,3- bis- Download PDFInfo
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- CN105837440B CN105837440B CN201610226969.XA CN201610226969A CN105837440B CN 105837440 B CN105837440 B CN 105837440B CN 201610226969 A CN201610226969 A CN 201610226969A CN 105837440 B CN105837440 B CN 105837440B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/24—Preparation of carboxylic acid esters by reacting carboxylic acids or derivatives thereof with a carbon-to-oxygen ether bond, e.g. acetal, tetrahydrofuran
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/09—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis
- C07C29/095—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis of esters of organic acids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/50—Preparation of compounds having groups by reactions producing groups
- C07C41/56—Preparation of compounds having groups by reactions producing groups by condensation of aldehydes, paraformaldehyde, or ketones
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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
- C07C51/54—Preparation of carboxylic acid anhydrides
- C07C51/56—Preparation of carboxylic acid anhydrides from organic acids, their salts, their esters or their halides, e.g. by carboxylation
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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
- C07C51/54—Preparation of carboxylic acid anhydrides
- C07C51/573—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
Abstract
The present invention relates to chemical industry or pharmaceutical fields, specifically one kind 1, the preparation process of the chloro- 2- acetyl group methoxy propane of 3- bis-, it is 1, it joined raw materials recovery in the conventional preparation techniques of the chloro- 2- acetyl group methoxy propane of 3- bis- and utilize technique, aceticanhydride is recycled first, afterwards by aceticanhydride and by-product acetic acid -1, ethyl alcohol is added in the mixture of 3- dichloro isopropyl ester, synthesizing ethyl acetate, so that the aceticanhydride end of reaction in by-product, the condition provided is hydrolyzed for by-product, the by-product without aceticanhydride is obtained after having distilled ethyl acetate, alkali is at this time added, by-product is hydrolyzed, obtain the 1 of crude product, 3=glycerin dichlorohydrin, by rectifying, 1, 3- glycerin dichlorohydrin can be used as starting material again and be produced, cost and environmental pollution are greatly reduced in this way, make Waste material is fully utilized and economic benefit.
Description
Technical field
The present invention relates to chemical industry or pharmaceutical fields, the specifically chloro- 2- acetyl group methoxy propyl of 1,3- of one kind bis-
The preparation process of alkane.
Background technique
1,3- bis- chloro- 2- acetyl group methoxy propane is the main intermediate of antivirus raw material medicine Ganciclovir, at home,
There is larger market in the world, at present in the preparation process of the chloro- 2- acetyl group methoxy propane of 1,3- bis-, is generally used dichloro
Glycerol, paraformaldehyde, aceticanhydride, the concentrated sulfuric acid carry out the conjunction of the chloro- 2- acetyl group methoxy propane of 1,3- bis- as main raw material
At wherein the most commonly used several synthesis technologies are as follows in the prior art:
(1) glycerin dichlorohydrin is put into reaction kettle, opens stirring, paraformaldehyde, p-methyl benzenesulfonic acid is added；In 1 hour slowly
Be warming up to 80 DEG C, and 85 ± 5 DEG C insulation reaction 3 ~ 5 hours；Benzene is added from head tank, heating carries out reflux water-dividing, when dividing water
Between 24 hours, still have a small amount of droplet in water segregator at this time；Air-distillation recycles benzene to 130 DEG C of interior temperature, then vacuum distillation recycling
Glycerin dichlorohydrin is steamed to about 130 DEG C of interior temperature, until steaming substantially without glycerin dichlorohydrin；60 DEG C are cooled to hereinafter, adding from head tank
Enter 95% ethyl alcohol or mother liquor, temperature rising reflux 30 minutes, then slowly cool to 0~5 DEG C, makes the crystallization of product acetal completely, centrifugation
Drying, is poured with ethanol in proper amount and is washed, continue to dry.
(2) reaction kettle is cleaned into drying, puts into acetal；70 DEG C are warming up to, remove ethyl alcohol under reduced pressure to 120 DEG C of kettle temperature and is protected
Temperature suction 30 minutes；50 DEG C are cooled to, aceticanhydride, sulfuric acid are sucked；Be warming up to 80 DEG C, 80 ± 5 DEG C insulation reaction 8 hours；It has kept the temperature
Potassium acetate or sodium acetate neutralisation of sulphuric acid is added in Bi Hou, stirs 30 minutes；Vacuum distillation recycles unreacted aceticanhydride to interior temperature 120
~125 DEG C, 95 DEG C of temperature, raffinate is cooled to 30 DEG C and is transferred to fractionation kettle, controls reflux ratio appropriate, and front-end volatiles are evaporated off and evaporate in
Point, regather positive fraction (116 DEG C/25mmHg, 106 DEG C/5mmHg, 110 DEG C/12mmHg).
(3) in clean dried reaction kettle, the chloro- 2- propyl alcohol of 1.3- bis-, paraformaldehyde, sulfuric acid is added, slowly heats up, in 2
Hour is warming up to 96-98 DEG C, keeps the temperature 2 hours, and heat preservation is finished, and cools to 10 DEG C and starts that aceticanhydride is added dropwise, and temperature is maintained at 15-20 DEG C,
It finishing, heating keeps the temperature 10 hours in 35-40 DEG C, and potassium acetate, stirring is added, and vacuum recycles aceticanhydride to 100 DEG C, is cooled to 20 DEG C,
Filtering, filtrate are pumped into rectifying still, and what is steamed under collection 115 DEG C/10mmHg state evaporates confusingly to get weight yield 80%, content
>=95% 2- chloroacetic chloride ylmethoxy -1.3- dichloropropane.This technology is application No. is the one of 201110253654.1
It is embodied in Chinese patent.
In above-mentioned several preparation processes, face that raw material availability and product yield are low to ask in actual production
Topic, and be the recycling referred to raw material in above-mentioned preparation process, cause using aforesaid way in processing,
Easily lead to defect at high cost, environmental pollution is serious.In consideration of it, the present invention provides the chloro- 2- acetyl group methoxies of 1,3- of one kind bis-
The preparation process of base propane joined raw material in the conventional preparation techniques of the chloro- 2- acetyl group methoxy propane of 1,3- bis- and return
Receive utilize technique, aceticanhydride is recycled first, after pass through the mixture to aceticanhydride and by-product acetic acid -1,3- dichloro isopropyl ester
Middle addition ethyl alcohol, the boiling point of synthesizing ethyl acetate, ethyl acetate is more much lower than by-product boiling point, and makes the vinegar in by-product
Anhydride reactant finishes, and hydrolyzes the condition provided for by-product, the by-product without aceticanhydride is obtained after having distilled ethyl acetate
Alkali is at this time added in object, and by-product is hydrolyzed, and obtains 1, the 3=glycerin dichlorohydrin of crude product, and by rectifying, 1,3- dichloro is sweet
Oil can be used as starting material again and be produced, and cost and environmental pollution be greatly reduced in this way, so that waste material obtains sufficiently
Utilization and economic benefit.
In the present invention, common technical terms are explained as follows, the abbreviation of mmHg, that is, millimeter of mercury, also known as millimeter mercury
Column, abbreviation millimeter (mm) is the unit that pressure, pressure value are directly indicated with the millimeter of mercury pressure, and principle is with mercury
Static pressure caused by column carrys out balancing Atmospheric pressure P, thus the height of mercury column can measure the size of atmospheric pressure, test
Room usually uses millimetres of mercury (mmHg) as the unit of atmospheric pressure.Reflux ratio refers to the ratio between regurgitant volume Lo and overhead product D,
That is: the size of R=Lo/D reflux ratio is according to the complexity (i.e. the size of relative volatility) of each component separation and to production
Depending on the requirement of quality.
Summary of the invention
In order to make up for the deficiencies of the prior art, the present invention provides the chloro- 2- acetyl group methoxy propanes of 1,3- of one kind bis-
Preparation process can be improved raw material availability and product in the preparation process of the chloro- 2- acetyl group methoxy propane of 1,3- bis-
Yield reduces the preparation cost of the chloro- 2- acetyl group methoxy propane of 1,3- bis-, reduces environmental pollution.
The technical solution adopted by the present invention to solve the technical problems is: the chloro- 2- acetyl group methoxy propyl of 1,3- of one kind bis-
The preparation process of alkane, it is characterised in that: specific step is as follows for the technique:
A. following substance is extracted by weight, glycerin dichlorohydrin, paraformaldehyde, the concentrated sulfuric acid devote in enamel gauging tank A,
It opens jacket steam and is heated to 75-85 DEG C, keep the temperature 3 hours, the chemical reaction carried out during this is shown below:
B. it is pumped into excessive aceticanhydride into enamel gauging tank, interior temperature is kept to add aceticanhydride in 10 hours, latter stirring heat preservation 8 hours,
The chemical reaction carried out during this is shown below:
C. after the completion of stirring, with reactant is pumped into rectifying still A by several times to PH4-5 in sodium acetate and in enamel gauging tank,
- 0.096Mpa first is boiled off with water punching pump, interior temperature control system fractionates out substance A in 100 DEG C or less progress fractions, only will in this step
Substance A largely distills；
D. after the completion of being fractionated, then second level lobe pump is increased, under conditions of 75 DEG C of control≤interior temperature≤83 DEG C/750mmHg, beaten
Reflux ratio boils off middle fraction, distills out substance B, and substance B is added in enamel gauging tank B, is then added into enamel gauging tank
Ethyl alcohol, after alkaline solution is added dropwise during stirring, stirred 2 hours after being added dropwise to complete, stirring after the completion of be pumped into rectifying still B
In, -0.096Mpa first is boiled off with water punching pump, interior temperature control system is fractionated between 78-85 DEG C, is fractionated out substance C, has been fractionated
Under conditions of Cheng Hou, 175 DEG C of control≤interior temperature≤180 DEG C/750mmHg, do not beat reflux ratio, fractionate out substance D, this in the process into
Capable chemical reaction is shown below:
(1) chemical reaction mainly occurred after ethyl alcohol is added
It is added after ethyl alcohol simultaneously with the chemical reaction occurred
(2) chemical reaction occurred after alkaline solution is added
E. substance A returns continues to use in b step, and substance D is returned to be continued to use in a step；
F. finally, not beating reflux ratio under conditions of 84 DEG C of control≤interior temperature≤125 DEG C/750mmHg, fractionating out substance i.e.
For the chloro- 2- acetyl group methoxy propane of 1,3- bis-；
Wherein: the A liquid is aceticanhydride；The substance B is the mixture of aceticanhydride and acetic acid -1,3- dichloro isopropyl ester
Matter；The substance C is ethyl acetate；The substance D is glycerin dichlorohydrin；By-product acetic acid -1,3- dichloro isopropyl
Ester is hydrolyzed to glycerin dichlorohydrin under alkaline environment, continues to use as raw material；Alkaline solution described in step d is NaOH
One of solution, KOH solution.
The beneficial effects of the present invention are: the present invention provides the preparations of the chloro- 2- acetyl group methoxy propane of 1,3- of one kind bis-
Technique joined raw materials recovery using technique, head in the conventional preparation techniques of the chloro- 2- acetyl group methoxy propane of 1,3- bis-
First aceticanhydride is recycled, after by the way that ethyl alcohol is added in the mixture to aceticanhydride and by-product acetic acid -1,3- dichloro isopropyl ester, close
At ethyl acetate, the boiling point of ethyl acetate is more much lower than by-product boiling point, and makes the aceticanhydride end of reaction in by-product, is
By-product hydrolyzes the condition provided, and the by-product without aceticanhydride is obtained after having distilled ethyl acetate, is at this time added
By-product is hydrolyzed alkali, obtains 1, the 3=glycerin dichlorohydrin of crude product, and by rectifying, 1,3- glycerin dichlorohydrin can be used as again
Beginning raw material is produced, and greatly reduces cost and environmental pollution in this way, so that waste material is fully utilized and economic effect
Benefit.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Embodiment is closed, the present invention is further explained.
Embodiment 1
By weight following substance is extracted, glycerin dichlorohydrin 226Kg, paraformaldehyde 50Kg, concentrated sulfuric acid 0.6L devote enamel
In measuring tank A, opens jacket steam and be heated to 75-85 DEG C, keep the temperature 3 hours；Then it is pumped into enamel gauging tank excessive
Aceticanhydride keeps interior temperature to add aceticanhydride 260L in 10 hours, and latter stirring heat preservation 8 hours；After the completion of stirring, in sodium acetate and enamel meter
Reactant is pumped into rectifying still A by several times to PH4-5, first boils off -0.096Mpa with water punching pump, interior temperature control system is at 100 DEG C in measuring tank
Fraction is carried out below, fractionates out extra aceticanhydride；After the completion of fractionation, then second level lobe pump is increased, 75 DEG C of control≤interior temperature≤83
DEG C/750mmHg under conditions of, beat reflux ratio, boil off middle fraction, distill out the mixing of aceticanhydride and acetic acid -1,3- dichloro isopropyl ester
Object adds the mixture in enamel gauging tank B, ethyl alcohol is then added into enamel gauging tank, after during stirring
The NaOH solution 200L of 2mol/L after being added dropwise to complete, is stirred 2 hours, is pumped into rectifying still B after the completion of stirring, first rushed and pumped with water
- 0.096Mpa is boiled off, interior temperature control system is fractionated between 78-85 DEG C, ethyl acetate is fractionated out, after the completion of fractionation, control
Under conditions of 175 DEG C≤interior temperature≤180 DEG C/750mmHg, reflux ratio is not beaten, substance glycerin dichlorohydrin is fractionated out；Aceticanhydride returns to b step
It is continued to use in rapid, glycerin dichlorohydrin returns to be continued to use in a step；Finally, 84 DEG C of control≤interior temperature≤125 DEG C/750mmHg
Under the conditions of, reflux ratio is not beaten, fractionating out substance is the chloro- 2- acetyl group methoxy propane of 1,3- bis-, and weight is obtained after weighing
372.7kg is 92.72% by glycerin dichlorohydrin calculated yield.
Embodiment 2
By weight following substance is extracted, glycerin dichlorohydrin 113Kg, paraformaldehyde 20Kg, concentrated sulfuric acid 0.6L devote enamel
In measuring tank A, opens jacket steam and be heated to 75-85 DEG C, keep the temperature 3 hours；Then it is pumped into enamel gauging tank excessive
Aceticanhydride keeps interior temperature to add aceticanhydride 180L in 10 hours, and latter stirring heat preservation 8 hours；After the completion of stirring, in sodium acetate and enamel meter
Reactant is pumped into rectifying still A by several times to PH4-5, first boils off -0.096Mpa with water punching pump, interior temperature control system is at 100 DEG C in measuring tank
Fraction is carried out below, fractionates out extra aceticanhydride；After the completion of fractionation, then second level lobe pump is increased, 75 DEG C of control≤interior temperature≤83
DEG C/750mmHg under conditions of, beat reflux ratio, boil off middle fraction, distill out the mixing of aceticanhydride and acetic acid -1,3- dichloro isopropyl ester
Object adds the mixture in enamel gauging tank B, ethyl alcohol is then added into enamel gauging tank, after during stirring
The NaOH solution 150L of 2mol/L after being added dropwise to complete, is stirred 2 hours, is pumped into rectifying still B after the completion of stirring, first rushed and pumped with water
- 0.096Mpa is boiled off, interior temperature control system is fractionated between 78-85 DEG C, ethyl acetate is fractionated out, after the completion of fractionation, control
Under conditions of 175 DEG C≤interior temperature≤180 DEG C/750mmHg, reflux ratio is not beaten, substance glycerin dichlorohydrin is fractionated out；Aceticanhydride returns to b step
It is continued to use in rapid, glycerin dichlorohydrin returns to be continued to use in a step；Finally, 84 DEG C of control≤interior temperature≤125 DEG C/750mmHg
Under the conditions of, reflux ratio is not beaten, fractionating out substance is the chloro- 2- acetyl group methoxy propane of 1,3- bis-, and weight is obtained after weighing
187.2kg is 93.14% by glycerin dichlorohydrin calculated yield.
Embodiment 3
By weight following substance is extracted, glycerin dichlorohydrin 170Kg, paraformaldehyde 40Kg, concentrated sulfuric acid 0.6L devote enamel
In measuring tank A, opens jacket steam and be heated to 75-85 DEG C, keep the temperature 3 hours；Then it is pumped into enamel gauging tank excessive
Aceticanhydride keeps interior temperature to add aceticanhydride 220L in 10 hours, and latter stirring heat preservation 8 hours；After the completion of stirring, in sodium acetate and enamel meter
Reactant is pumped into rectifying still A by several times to PH4-5, first boils off -0.096Mpa with water punching pump, interior temperature control system is at 100 DEG C in measuring tank
Fraction is carried out below, fractionates out extra aceticanhydride；After the completion of fractionation, then second level lobe pump is increased, 75 DEG C of control≤interior temperature≤83
DEG C/750mmHg under conditions of, beat reflux ratio, boil off middle fraction, distill out the mixing of aceticanhydride and acetic acid -1,3- dichloro isopropyl ester
Object adds the mixture in enamel gauging tank B, ethyl alcohol is then added into enamel gauging tank, after during stirring
The KOH solution 180L of 2mol/L after being added dropwise to complete, is stirred 2 hours, is pumped into rectifying still B after the completion of stirring, is first rushed pump with water and is steamed
- 0.096Mpa is removed, interior temperature control system is fractionated between 78-85 DEG C, ethyl acetate is fractionated out, after the completion of fractionation, control 175
DEG C≤interior temperature≤180 DEG C/750mmHg under conditions of, do not beat reflux ratio, fractionate out substance glycerin dichlorohydrin；Aceticanhydride returns in b step
It continues to use, glycerin dichlorohydrin returns to be continued to use in a step；Finally, 84 DEG C of control≤interior temperature≤125 DEG C/750mmHg condition
Under, reflux ratio is not beaten, fractionating out substance is the chloro- 2- acetyl group methoxy propane of 1,3- bis-, weight 277.2kg is obtained after weighing,
It is 91.68% by glycerin dichlorohydrin calculated yield.
Embodiment 4
By weight following substance is extracted, glycerin dichlorohydrin 226Kg, paraformaldehyde 50Kg, concentrated sulfuric acid 0.6L devote enamel
In measuring tank A, opens jacket steam and be heated to 75-85 DEG C, keep the temperature 3 hours；Then it is pumped into enamel gauging tank excessive
Aceticanhydride keeps interior temperature to add aceticanhydride 260L in 10 hours, and latter stirring heat preservation 8 hours；After the completion of stirring, in sodium acetate and enamel meter
Reactant is pumped into rectifying still A by several times to PH4-5, first boils off -0.096Mpa with water punching pump, interior temperature control system is at 100 DEG C in measuring tank
Fraction is carried out below, fractionates out extra aceticanhydride；After the completion of fractionation, then second level lobe pump is increased, 75 DEG C of control≤interior temperature≤83
DEG C/750mmHg under conditions of, beat reflux ratio, boil off middle fraction, distill out the mixing of aceticanhydride and acetic acid -1,3- dichloro isopropyl ester
Object adds the mixture in enamel gauging tank B, ethyl alcohol is then added into enamel gauging tank, after during stirring
The KOH solution 200L of 2mol/L after being added dropwise to complete, is stirred 2 hours, is pumped into rectifying still B after the completion of stirring, is first rushed pump with water and is steamed
- 0.096Mpa is removed, interior temperature control system is fractionated between 78-85 DEG C, ethyl acetate is fractionated out, after the completion of fractionation, control 175
DEG C≤interior temperature≤180 DEG C/750mmHg under conditions of, do not beat reflux ratio, fractionate out substance glycerin dichlorohydrin；Aceticanhydride returns in b step
It continues to use, glycerin dichlorohydrin returns to be continued to use in a step；Finally, 84 DEG C of control≤interior temperature≤125 DEG C/750mmHg condition
Under, reflux ratio is not beaten, fractionating out substance is the chloro- 2- acetyl group methoxy propane of 1,3- bis-, weight 375.4kg is obtained after weighing,
It is 93.38% by glycerin dichlorohydrin calculated yield.
The basic principles, main features and advantages of the invention have been shown and described above.The technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and only illustrating for the description in above embodiments and description is of the invention
Principle, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these change and change
Into all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by appended claims and its equivalent
It defines.
Claims (1)
1. the preparation process of the chloro- 2- acetyl group methoxy propane of 1,3- of one kind bis-, it is characterised in that: the specific steps of the technique are such as
Under:
A. following substance is extracted by weight, and glycerin dichlorohydrin, paraformaldehyde, the concentrated sulfuric acid devote in enamel gauging tank A, open
Jacket steam is heated to 75-85 DEG C, keeps the temperature 3 hours；
B. it is pumped into excessive aceticanhydride into enamel gauging tank A, interior temperature is kept to add aceticanhydride in 10 hours, latter stirring heat preservation 8 hours；
C. after the completion of stirring, with reactant is pumped into rectifying still A, first by several times to PH4-5 in sodium acetate and in enamel gauging tank A
- 0.096Mpa is boiled off with water punching pump, interior temperature control system is at 100 DEG C hereinafter, progress fraction, fractionates out substance A；
D. after the completion of being fractionated, then second level lobe pump is increased, under conditions of 75 DEG C of control≤interior temperature≤83 DEG C/750mmHg, returns stream
Than boiling off middle fraction, distilling out substance B, substance B is added in enamel gauging tank B, second then is added into enamel gauging tank B
Alcohol, after alkaline solution is added dropwise during stirring, stirred 2 hours after being added dropwise to complete, stirring after the completion of be pumped into rectifying still B in,
- 0.096Mpa first is boiled off with water punching pump, interior temperature control system is fractionated between 78-85 DEG C, fractionates out substance C, and fractionation is completed
Afterwards, under conditions of 175 DEG C of control≤interior temperature≤180 DEG C/750mmHg, reflux ratio is not beaten, substance D is fractionated out；
E. substance A returns continues to use in b step, and substance D is returned to be continued to use in a step；
F. finally, not beating reflux ratio under conditions of 84 DEG C of control≤interior temperature≤125 DEG C/750mmHg, fractionating out substance is 1,
The chloro- 2- acetyl group methoxy propane of 3- bis-；
Wherein: the substance A is aceticanhydride；The substance B is the compounding substances of aceticanhydride and acetic acid -1,3- dichloro isopropyl ester；Institute
The substance C stated is ethyl acetate；The substance D is glycerin dichlorohydrin；Acetic acid -1,3- dichloro isopropyl ester is under alkaline environment by water
Solution is glycerin dichlorohydrin, is continued to use as raw material；Alkaline solution described in step d is NaOH solution, one in KOH solution
Kind.
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| CN103804192A (en) * | 2014-02-18 | 2014-05-21 | 安徽海康药业有限责任公司 | Method for preparing 1, 3-dihalogenated-2-propoxy methyl alcohol alkyl carboxylic ester |
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| CN102952017A (en) * | 2011-08-24 | 2013-03-06 | 湖北保乐制药有限公司 | Preparation method of 2-acetylchloromethoxy-1,3-dichloropropane |
| CN103130642A (en) * | 2011-11-30 | 2013-06-05 | 湖北保乐制药有限公司 | Preparation method of 2-acetoxyl group methoxy group-1.3-propylene dichloride |
| CN102702199A (en) * | 2012-06-13 | 2012-10-03 | 湖北葛店人福药业有限责任公司 | Method for preparing ganciclovir |
| CN103804192A (en) * | 2014-02-18 | 2014-05-21 | 安徽海康药业有限责任公司 | Method for preparing 1, 3-dihalogenated-2-propoxy methyl alcohol alkyl carboxylic ester |
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