CN105859559A - Production method of 3-ethoxy-4-nitrophenol - Google Patents
Production method of 3-ethoxy-4-nitrophenol Download PDFInfo
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- CN105859559A CN105859559A CN201610273580.0A CN201610273580A CN105859559A CN 105859559 A CN105859559 A CN 105859559A CN 201610273580 A CN201610273580 A CN 201610273580A CN 105859559 A CN105859559 A CN 105859559A
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- C07—ORGANIC CHEMISTRY
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- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/08—Preparation of nitro compounds by substitution of hydrogen atoms by nitro groups
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- C07—ORGANIC CHEMISTRY
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- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
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Abstract
The invention discloses a production method of 3-ethoxy-4-nitrophenol. The low-price m-dichlorobenzene is used instead of the high-price resorcinol as the raw material, and the methoxy is converted into the hydroxy; and a simple alkaline process is used instead of the conventional hydrogen bromide/acetic acid system to prepare the 3-ethoxy-4-nitrophenol. By using low-price m-dichlorobenzene instead of the high-price resorcinol as the raw material to prepare the 3-ethoxy-4-nitrophenol, the method has the advantages of simple synthesis steps, low pollution, environment friendliness, high product quality, high yield, low production cost and normal-pressure operation, and can implement industrial production.
Description
Technical field
The invention belongs to chemical material technical field, more particularly, it relates to a kind of 3-ethyoxyl-4-nitrobenzene
The production method of phenol.
Background technology
Oxyfluorfen [the chloro-1-of 2-(3-ethyoxyl-4-nitrophenoxy)-4-trifluoromethylbenzene] is state in recent years
The interior new environment-friendly type diphenyl ether herbicide emerged, it is wide that it has herbicidal spectrum, and weeding ratio is high, noresidue, substantially
Nontoxicity, the advantages such as mu dosage is few, and agriculture is the lowest, development prospect is the most good.3-ethyoxyl-4-nitrobenzene
Phenol is the important intermediate of synthesizing oxyfluorfen, and synthetic reaction formula is:
3-ethyoxyl-4-nitrophenol production method is mainly with resorcinol as raw material at present, employing bis ether method,
Etherified hydroxyl protection method or the synthesis of etherified hydroxyl protection method prepare, and these methods exist process route length, former
The defects such as material price is high, product content is low, cost is high, environmental pollution is serious.Also it is former for having with 3-chlorophenol
Material, generates intermediate 3-chloro-4-nitrophenol through nitration reaction, then generates 3-ethyoxyl-4-through condensation reaction
Nitrophenol, but 3-chlorophenol source is few, and price is high, and industrial production cost is high.
Therefore, select that a kind of synthesis step is simple, excellent good, the low cost of environmental protection, product quality, can industry
3-ethyoxyl-4-nitrophenol the preparation method that metaplasia is produced, its meaning is outstanding.
Summary of the invention
1, problem to be solved
For the above-mentioned problems in the prior art, the present invention provides a kind of production cost low, atmospheric operation,
Polluting low, yield is high, a kind of production method of the 3-ethyoxyl-4-nitrophenol that product content is high, to solve
The problem that above-mentioned prior art is not enough.
2, technical scheme
In order to solve the problems referred to above, the technical solution adopted in the present invention is as follows:
The production method of a kind of 3-ethyoxyl-4-nitrophenol, described production method comprises the steps:
(1) to the nitration mixture being configured to according to a certain ratio equipped with the concentrated sulfuric acid and nitric acid under room temperature and strong agitation effect
Flask one in drip m-dichlorobenzene, time for adding is 1.5-2h, meets and be incubated under the conditions of 60 DEG C after being added dropwise to complete
Reaction 1h；
(2) divide spent acid by step (1) products therefrom, then under room temperature condition, be washed till neutrality with light buck,
Then at 100 DEG C with the NaOH solution of 20% be washed till dinitro compound disappear, cold filtration be dried 2,4-bis-
Chloronitrobenzene；
(3) by step (2) gained 2,4-dichloronitrobenzene is dissolved in the solvent one being contained in flask two, and
Dripping sodium methoxide solution at room temperature in described flask two, time for adding is 0.5h, under reflux conditions reacts
5-6h；
(4) step (3) products therefrom steaming solvent one, add water, stirred crystallization filters, with solvent one
Recrystallization, obtains 2-chloro-4-methoxy nitrobenzene pale yellow crystals after filtration drying；
(5) step (4) gained 2-chloro-4-methoxy nitrobenzene and KOH solution are added in flask three, then
Adding consisting of phase-transferring agent, back flow reaction 15 hours under the conditions of 105-115 DEG C, until all dissolving；
(6) in step (5) products therefrom, add hydrochloric acid acidifying, separate out 2-chloro-4-hydroxyl nitrobenzene, filter and dry
2-chloro-4-hydroxyl nitrobenzene yellow solid is obtained after Gan；
(7) step (6) gained 2-chloro-4-hydroxyl nitrobenzene is dissolved in the solvent two being contained in flask four,
And in described flask four, dripping alcohol sodium solution at room temperature, time for adding is 0.5h, the most instead
Answer 5-6h；
(8) decompression in step (7) products therefrom is steamed solvent two, be subsequently adding the hydrochloric acid acidifying of 10%, stir
Mix crystallization to filter, remove salt solution, wash filter cake with water, obtain 3-ethyoxyl-4-nitrophenol crystal.
Preferably, described flask one, flask two, flask three are the most identical with flask four, and are all and stir equipped with machinery
Mix, dropping funel and the there-necked flask of reflux condensing tube.
Preferably, nitric acid described in described step (1) be mass fraction be the fuming nitric aicd of 96.5%, described dense
The mass fraction of sulfuric acid is 98%；The amount of described nitric acid and the material of the concentrated sulfuric acid is than for 1.05:1, described nitric acid
With the amount of the material of m-dichlorobenzene than for 1.2:1.
Preferably, described in step (4), solvent one is methyl alcohol, described sodium methoxide and 2,4-dichloronitrobenzene
The amount of material is 1.05:1.
Preferably, described in step (5), the mass fraction of KOH solution is 40%, the chloro-4-of described KOH Yu 2-
The amount of the material of methoxy nitrobenzene is than for 2.5:1, and described consisting of phase-transferring agent is PEG400, and described consisting of phase-transferring agent
The 3-5% that addition is described 2-chloro-4-methoxy nitrobenzene consumption.
Preferably, described in step (7), solvent two is ethanol, described caustic alcohol and 2-chloro-4-hydroxyl nitrobenzene
The amount of material compare 2.05:1.
Preferably, the solvent two that in the solvent one steamed in described step (3) and step (7), decompression steams is equal
Can circulate and re-use.
3, beneficial effect
Compared to prior art, the invention have the benefit that
(1) resorcinol that the present invention uses cheap m-dichlorobenzene to substitute high price is raw material, prepares 3-
Ethyoxyl-4-nitrophenol, it has, and synthesis step is simple, pollute low environmental protection, product quality is high, receipts
Rate is high, production cost is low, atmospheric operation, can the advantage of industrialized production；
(2) methoxyl group is converted into hydroxyl reaction by the present invention, uses easy alkaline process, replaces conventional hydrogen bromide
/ acetate system, saves a large amount of expense, eliminates the problem of environmental pollution of hydrogen bromide simultaneously；
(3) overall yield of reaction of the present invention is up to 78%, and the purity of prepared 3-ethyoxyl-4-nitrophenol
More than 95%.
Accompanying drawing explanation
Fig. 1 is the production method synthetic route chart of a kind of 3-ethyoxyl-4-nitrophenol of the present invention.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further described below.
Embodiment 1
The production method of a kind of 3-ethyoxyl-4-nitrophenol, specifically includes following steps:
(1) under room temperature, the fuming nitric aicd of 39g concentration 96.5%, the sulfuric acid of 57g concentration 98% are weighed, preparation
Become nitration mixture, equipped with in the 500ml there-necked flask of mechanical agitation, dropping funel and reflux condensing tube, add 75g
The m-dichlorobenzene of concentration 98%, drips nitration mixture under the conditions of strong agitation, and time for adding is 1.5-2 hour, adds
After complete at 60 DEG C insulation reaction 1 hour, after point removing spent acid, under room temperature condition, light buck is washed till neutrality,
Being washed till dinitro compound with 20%NaOH solution at 100 DEG C to disappear, crystallisation by cooling, filtration drying 93.2g is faint yellow
Obtaining 2,4-dichloronitrobenzene solid, recording content is 98.3%, and yield is 95.4%.
(2) equipped with in the 500ml there-necked flask of mechanical agitation, dropping funel and reflux condensing tube, 98g is added
The 2 of concentration 98%, 4-dichloronitrobenzene and 200g absolute methanol, stirring is by 2, and 4-dichloronitrobenzene is dissolved in methyl alcohol
In solution, drip the sodium methoxide solution of 95g concentration 30% at ambient temperature, within 0.5 hour, drip off, at 68 DEG C
Reacting 5-6 hour under the counterflow condition of left and right, after reaction terminates, it is (capable of circulation after methyl alcohol abjection that normal pressure steams methyl alcohol
Use), add washing and desalt, stirred crystallization filters, and with 200g methyl alcohol, product recrystallizes (mother liquor steaming
After going out methyl alcohol, methanol loop uses), filtration drying obtains 84.2g2-chloro-4-methoxy nitrobenzene pale yellow crystals,
Recording content is 95.2%, and yield is 85.5%.
(3) equipped with in the 500ml there-necked flask of mechanical agitation, dropping funel and reflux condensing tube, 99g is added
Content 95%2-chloro-4-methoxy nitrobenzene solid, 350g20%KOH solution and 3g PEG400, agitating heating,
110 DEG C of back flow reaction about 15 hours, after all dissolving to solid, add hydrochloric acid acidifying, separate out the chloro-4-of 2-
Hydroxyl nitrobenzene, after filtering drying, obtains 82.5g2-chloro-4-hydroxyl nitrobenzene yellow solid, records content 95.2%,
Yield is 90.5%.
(4) equipped with in the 1000ml there-necked flask of mechanical agitation, dropping funel and reflux condensing tube, add
91g2-chloro-4-hydroxyl nitrobenzene solid, 200g absolute ethyl alcohol, stirring makes 2-chloro-4-hydroxyl nitrobenzene be dissolved in second
In alcoholic solution, dropping 348g20% alcohol sodium solution, drips off, on 78 DEG C of left sides for about 0.5 hour at ambient temperature
Reacting 5-6 hour under right counterflow condition, after reaction terminates, decompression steams ethanol (ethanol abjection Posterior circle uses),
Being subsequently adding washing to desalt, then be acidified with 10% hydrochloric acid, stirred crystallization, filtration drying obtains 94.5g product 3-
Ethyoxyl-4-nitrophenol crystal, recording content is 95.4%, and yield is 98.5%.
Embodiment 2
(1) under room temperature, the fuming nitric aicd of 39g concentration 96.5%, the sulfuric acid of 57g concentration 98% are weighed, preparation
Become nitration mixture, equipped with in the 500ml there-necked flask of mechanical agitation, dropping funel and reflux condensing tube, add 75g
The m-dichlorobenzene of concentration 98%, drips nitration mixture under the conditions of strong agitation, and time for adding is 1.5-2 hour, adds
After complete at 60 DEG C insulation reaction 1 hour, after point removing spent acid, under room temperature condition, light buck is washed till neutrality,
Being washed till dinitro compound with 20%NaOH solution at 100 DEG C to disappear, crystallisation by cooling, filtration drying 93.2g is faint yellow
Obtaining 2,4-dichloronitrobenzene solid, recording content is 98.3%, and yield is 95.4%.
(2) equipped with in the 500ml there-necked flask of mechanical agitation, dropping funel and reflux condensing tube, 98g is added
The 2 of concentration 98%, 4-dichloronitrobenzene and 200g absolute methanol, stirring is by 2, and 4-dichloronitrobenzene is dissolved in methyl alcohol
In solution, drip the sodium methoxide solution of 95g concentration 30% at ambient temperature, within 0.5 hour, drip off, at 68 DEG C
Reacting 5-6 hour under the counterflow condition of left and right, after reaction terminates, it is (capable of circulation after methyl alcohol abjection that normal pressure steams methyl alcohol
Use), add washing and desalt, stirred crystallization filters, and with 200g methyl alcohol, product recrystallizes (mother liquor steaming
After going out methyl alcohol, methanol loop uses), filtration drying obtains 84.2g2-chloro-4-methoxy nitrobenzene pale yellow crystals,
Recording content is 95.2%, and yield is 85.5%.
(3) equipped with in the 500ml there-necked flask of mechanical agitation, dropping funel and reflux condensing tube, 99g is added
Content 95%2-chloro-4-methoxy nitrobenzene solid, 235g30%KOH solution and 3g PEG400, agitating heating,
110 DEG C of back flow reaction about 15 hours, after all dissolving to solid, add hydrochloric acid acidifying, separate out the chloro-4-of 2-
Hydroxyl nitrobenzene, after filtering drying, obtains 83.8g2-chloro-4-hydroxyl nitrobenzene yellow solid, records content
95.8%, yield is 92.5%.
(4) equipped with in the 1000ml there-necked flask of mechanical agitation, dropping funel and reflux condensing tube, add
91g2-chloro-4-hydroxyl nitrobenzene solid, 200g absolute ethyl alcohol, stirring makes 2-chloro-4-hydroxyl nitrobenzene be dissolved in second
In alcoholic solution, dropping 348g20% alcohol sodium solution, drips off, on 78 DEG C of left sides for about 0.5 hour at ambient temperature
Reacting 5-6 hour under right counterflow condition, after reaction terminates, decompression steams ethanol (ethanol abjection Posterior circle uses),
Being subsequently adding washing to desalt, then be acidified with 10% hydrochloric acid, stirred crystallization, filtration drying obtains 94.5g product 3-
Ethyoxyl-4-nitrophenol crystal, recording content is 95.4%, and yield is 98.5%.
Embodiment 3
(1) under room temperature, the fuming nitric aicd of 39g concentration 96.5%, the sulfuric acid of 57g concentration 98% are weighed, preparation
Become nitration mixture, equipped with in the 500ml there-necked flask of mechanical agitation, dropping funel and reflux condensing tube, add 75g
The m-dichlorobenzene of concentration 98%, drips nitration mixture under the conditions of strong agitation, and time for adding is 1.5-2 hour, adds
After complete at 60 DEG C insulation reaction 1 hour, after point removing spent acid, under room temperature condition, light buck is washed till neutrality,
Being washed till dinitro compound with 20%NaOH solution at 100 DEG C to disappear, crystallisation by cooling, filtration drying 93.2g is faint yellow
Obtaining 2,4-dichloronitrobenzene solid, recording content is 98.3%, and yield is 95.4%.
(2) equipped with in the 500ml there-necked flask of mechanical agitation, dropping funel and reflux condensing tube, 98g is added
The 2 of concentration 98%, 4-dichloronitrobenzene and 200g absolute methanol, stirring is by 2, and 4-dichloronitrobenzene is dissolved in methyl alcohol
In solution, drip the sodium methoxide solution of 95g concentration 30% at ambient temperature, within 0.5 hour, drip off, at 68 DEG C
Reacting 5-6 hour under the counterflow condition of left and right, after reaction terminates, it is (capable of circulation after methyl alcohol abjection that normal pressure steams methyl alcohol
Use), add washing and desalt, stirred crystallization filters, and with 200g methyl alcohol, product recrystallizes (mother liquor steaming
After going out methyl alcohol, methanol loop uses), filtration drying obtains 84.2g2-chloro-4-methoxy nitrobenzene pale yellow crystals,
Recording content is 95.2%, and yield is 85.5%.
(3) equipped with in the 500ml there-necked flask of mechanical agitation, dropping funel and reflux condensing tube, 99g is added
Content 95%2-chloro-4-methoxy nitrobenzene solid, 175g40%KOH solution and 3g PEG400, agitating heating,
110 DEG C of back flow reaction about 15 hours, after all dissolving to solid, add hydrochloric acid acidifying, separate out the chloro-4-of 2-
Hydroxyl nitrobenzene, after filtering drying, obtains 88.7g2-chloro-4-hydroxyl nitrobenzene yellow solid, records content 96.0%,
Yield is 98.2%.
(4) equipped with in the 1000ml there-necked flask of mechanical agitation, dropping funel and reflux condensing tube, add
91g2-chloro-4-hydroxyl nitrobenzene solid, 200g absolute ethyl alcohol, stirring makes 2-chloro-4-hydroxyl nitrobenzene be dissolved in second
In alcoholic solution, dropping 348g20% alcohol sodium solution, drips off, on 78 DEG C of left sides for about 0.5 hour at ambient temperature
Reacting 5-6 hour under right counterflow condition, after reaction terminates, decompression steams ethanol (ethanol abjection Posterior circle uses),
Being subsequently adding washing to desalt, then be acidified with 10% hydrochloric acid, stirred crystallization, filtration drying obtains 94.5g product 3-
Ethyoxyl-4-nitrophenol crystal, recording content is 95.4%, and yield is 98.5%.
Embodiment 4
(1) under room temperature, the fuming nitric aicd of 39g concentration 96.5%, the sulfuric acid of 57g concentration 98% are weighed, preparation
Become nitration mixture, equipped with in the 500ml there-necked flask of mechanical agitation, dropping funel and reflux condensing tube, add 75g
The m-dichlorobenzene of concentration 98%, drips nitration mixture under the conditions of strong agitation, and time for adding is 1.5-2 hour, adds
After complete at 60 DEG C insulation reaction 1 hour, after point removing spent acid, under room temperature condition, light buck is washed till neutrality,
Being washed till dinitro compound with 20%NaOH solution at 100 DEG C to disappear, crystallisation by cooling, filtration drying 93.2g is faint yellow
Obtaining 2,4-dichloronitrobenzene solid, recording content is 98.3%, and yield is 95.4%.
(2) equipped with in the 500ml there-necked flask of mechanical agitation, dropping funel and reflux condensing tube, 98g is added
The 2 of concentration 98%, 4-dichloronitrobenzene and 200g absolute methanol, stirring is by 2, and 4-dichloronitrobenzene is dissolved in methyl alcohol
In solution, drip the sodium methoxide solution of 95g concentration 30% at ambient temperature, within 0.5 hour, drip off, at 68 DEG C
Reacting 5-6 hour under the counterflow condition of left and right, after reaction terminates, it is (capable of circulation after methyl alcohol abjection that normal pressure steams methyl alcohol
Use), add washing and desalt, stirred crystallization filters, and with 200g methyl alcohol, product recrystallizes (mother liquor steaming
After going out methyl alcohol, methanol loop uses), filtration drying obtains 84.2g2-chloro-4-methoxy nitrobenzene pale yellow crystals,
Recording content is 95.2%, and yield is 85.5%.
(3) equipped with in the 500ml there-necked flask of mechanical agitation, dropping funel and reflux condensing tube, 99g is added
Content 95%2-chloro-4-methoxy nitrobenzene solid, 140g50%KOH solution and 3g PEG400, agitating heating,
About 110 DEG C back flow reaction about 15 hours, after all dissolving to solid, add hydrochloric acid acidifying, separate out 2-
Chloro-4-hydroxyl nitrobenzene, after filtering drying, obtains 87.6g2-chloro-4-hydroxyl nitrobenzene yellow solid, records and contain
Amount 95.5%, yield is 96.4%.
(4) equipped with in the 1000ml there-necked flask of mechanical agitation, dropping funel and reflux condensing tube, add
91g2-chloro-4-hydroxyl nitrobenzene solid, 200g absolute ethyl alcohol, stirring makes 2-chloro-4-hydroxyl nitrobenzene be dissolved in second
In alcoholic solution, dropping 348g20% alcohol sodium solution, drips off, on 78 DEG C of left sides for about 0.5 hour at ambient temperature
Reacting 5-6 hour under right counterflow condition, after reaction terminates, decompression steams ethanol (ethanol abjection Posterior circle uses),
Being subsequently adding washing to desalt, then be acidified with 10% hydrochloric acid, stirred crystallization, filtration drying obtains 94.5g product 3-
Ethyoxyl-4-nitrophenol crystal, recording content is 95.4%, and yield is 98.5%.
Based on above-mentioned, the resorcinol that the present invention uses cheap m-dichlorobenzene to substitute high price is raw material,
Preparation 3-ethyoxyl-4-nitrophenol, it has, and synthesis step is simple, pollute low environmental protection, product quality
High, yield high, production cost is low, atmospheric operation, can the advantage of industrialized production；And by methoxyl group is turned
Turn to hydroxyl reaction, use easy alkaline process, replace conventional hydrogen bromide/acetate system, save a large amount of expense,
Eliminate the problem of environmental pollution of hydrogen bromide simultaneously；Overall yield of reaction of the present invention is up to 78%, and prepared 3-
The purity of ethyoxyl-4-nitrophenol is more than 95%.
Schematically being described the present invention and embodiment thereof above, this description is the most restricted.So,
If those of ordinary skill in the art is enlightened by it, in the case of without departing from the invention objective, without
Creative designs the frame mode embodiment similar to this technical scheme, all should belong to the protection model of the present invention
Enclose.
Claims (7)
1. the production method of a 3-ethyoxyl-4-nitrophenol, it is characterised in that described production method includes
Following steps:
(1) to the nitration mixture being configured to according to a certain ratio equipped with the concentrated sulfuric acid and nitric acid under room temperature and strong agitation effect
Flask one in drip m-dichlorobenzene, time for adding is 1.5-2h, meets and be incubated under the conditions of 60 DEG C after being added dropwise to complete
Reaction 1h；
(2) divide spent acid by step (1) products therefrom, then under room temperature condition, be washed till neutrality with light buck,
Then at 100 DEG C with the NaOH solution of 20% be washed till dinitro compound disappear, cold filtration be dried 2,4-bis-
Chloronitrobenzene；
(3) by step (2) gained 2,4-dichloronitrobenzene is dissolved in the solvent one being contained in flask two, and
Dripping sodium methoxide solution at room temperature in described flask two, time for adding is 0.5h, under reflux conditions reacts
5-6h；
(4) step (3) products therefrom steaming solvent one, add water, stirred crystallization filters, with solvent one
Recrystallization, obtains 2-chloro-4-methoxy nitrobenzene pale yellow crystals after filtration drying；
(5) step (4) gained 2-chloro-4-methoxy nitrobenzene and KOH solution are added in flask three, then
Adding consisting of phase-transferring agent, back flow reaction 15 hours under the conditions of 105-115 DEG C, until all dissolving；
(6) in step (5) products therefrom, add hydrochloric acid acidifying, separate out 2-chloro-4-hydroxyl nitrobenzene, filter and dry
2-chloro-4-hydroxyl nitrobenzene yellow solid is obtained after Gan；
(7) step (6) gained 2-chloro-4-hydroxyl nitrobenzene is dissolved in the solvent two being contained in flask four,
And in described flask four, dripping alcohol sodium solution at room temperature, time for adding is 0.5h, the most instead
Answer 5-6h；
(8) decompression in step (7) products therefrom is steamed solvent two, be subsequently adding the hydrochloric acid acidifying of 10%, stir
Mix crystallization to filter, remove salt solution, wash filter cake with water, obtain 3-ethyoxyl-4-nitrophenol crystal.
The production method of a kind of 3-ethyoxyl-4-nitrophenol the most according to claim 1, its feature exists
In, described flask one, flask two, flask three are the most identical with flask four, and are all equipped with mechanical agitation, dropping liquid
Funnel and the there-necked flask of reflux condensing tube.
The production method of a kind of 3-ethyoxyl-4-nitrophenol the most according to claim 1, its feature exists
In, nitric acid described in described step (1) be mass fraction be the fuming nitric aicd of 96.5%, the matter of the described concentrated sulfuric acid
Amount mark is 98%；The amount of described nitric acid and the material of the concentrated sulfuric acid is than for 1.05:1, described nitric acid and a dichloro
The amount of the material of benzene is than for 1.2:1.
The production method of a kind of 3-ethyoxyl-4-nitrophenol the most according to claim 1, its feature exists
In, described in step (4), solvent one is methyl alcohol, described sodium methoxide and 2, the amount of the material of 4-dichloronitrobenzene
For 1.05:1.
The production method of a kind of 3-ethyoxyl-4-nitrophenol the most according to claim 1, its feature exists
In, described in step (5), the mass fraction of KOH solution is 40%, described KOH Yu 2-chloro-4-methoxy nitre
The amount of the material of base benzene is than for 2.5:1, and described consisting of phase-transferring agent is PEG400, and the addition of described consisting of phase-transferring agent
3-5% for described 2-chloro-4-methoxy nitrobenzene consumption.
The production method of a kind of 3-ethyoxyl-4-nitrophenol the most according to claim 1, its feature exists
In, described in step (7), solvent two is ethanol, the material of described caustic alcohol and 2-chloro-4-hydroxyl nitrobenzene
Amount compares 2.05:1.
The production method of a kind of 3-ethyoxyl-4-nitrophenol the most according to claim 1, its feature exists
In, the solvent two that in the solvent one steamed in described step (3) and step (7), decompression steams all can circulate
Re-use.
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Cited By (2)
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| CN115108915A (en) * | 2022-06-17 | 2022-09-27 | 四川九原程新材料有限公司 | Preparation method of 1,3, 5-triethoxy-2, 4, 6-trinitrobenzene |
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| CN107417652A (en) * | 2017-04-13 | 2017-12-01 | 安徽广信农化股份有限公司 | A kind of synthesis technique of azoxystrobin intermediate benzofuranone |
| CN115108915A (en) * | 2022-06-17 | 2022-09-27 | 四川九原程新材料有限公司 | Preparation method of 1,3, 5-triethoxy-2, 4, 6-trinitrobenzene |
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