CN108707078A - A kind of production method of the o-nitrobenzaldehyde based on potassium ethoxide/niobium - Google Patents
A kind of production method of the o-nitrobenzaldehyde based on potassium ethoxide/niobium Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- 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
- C07C201/12—Preparation of nitro compounds by reactions not involving the formation of nitro groups
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Abstract
The present invention provides a kind of production method of the o-nitrobenzaldehyde based on potassium ethoxide/niobium, includes the following steps：Under nitrogen atmosphere, potassium is added in hexamethylene, ultrasonication, the benzole soln of niobium chloride is added, ethyl alcohol is added dropwise under cryogenic, continue supersonic oscillations, filtered, removed benzene, obtain the cyclohexane solution of potassium ethoxide/niobium；Ortho-methylnitrobenzene and diethy-aceto oxalate are added to the cyclohexane solution of potassium ethoxide/niobium, slow heating stirring to aneroid evacuator body complete to dissolving is stirred at room temperature, room temperature is down in stirring, after being washed with hexamethylene, drying obtains ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt；Under nitrogen light protected environment, ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt is added portionwise to the in the mixed solvent of hydrogen peroxide and hexamethylene, water is added dropwise, stirs at low ambient temperatures, filters layering, vacuum drying obtains o-nitrobenzaldehyde.Preparation method of the present invention is simple, and reaction condition is mild, efficient, the high income of yield, and purity is high.
Description
Technical field
The invention belongs to medicinal chemistry arts, and in particular to a kind of production of the o-nitrobenzaldehyde based on potassium ethoxide/niobium
Method.
Background technology
O-nitrobenzaldehyde abbreviation ONBD, is a kind of pale yellow powder crystal or glassy yellow acicular crystal, can be with water vapour
Volatilization, is soluble in the organic solvents such as ethyl alcohol, ether, benzene, easily by the dioxygen oxidation in air, o-nitrobenzaldehyde is a kind of heavy
The medicine and organic synthesis intermediate wanted are synthesis cardiovascular disease medicine nifedipine, Nisoldipine, encainide etc., eliminating the phlegm
The important intermediate of medicine ambroxol hydrochloride parent 3,5- dibromo o-Aminobenzaldehydes.
The preparation method of ortho-methylnitrobenzene aldehyde can by nitro alcohol, ortho-methylnitrobenzene, adjacent nitro benzyl halogen, benzaldehyde,
O-nitrobenzaldehyde, o-chlorobenzaldehyde synthesize to obtain, wherein be most widely used with the oxidation of aldehydes method of ortho-methylnitrobenzene, but adjacent nitre
Nitrotoleune is more unstable near base tolyl aldehyde, is easily aoxidized, it is therefore desirable to which control reaction rests on the o-nitrobenzaldehyde stage.
The method that bionically catalyzing and oxidizing ortho-methylnitrobenzene prepares o-nitrobenzaldehyde disclosed in Chinese patent CN 1243717C, with
Ortho-methylnitrobenzene is raw material, with the metal phthalein mountain valley with clumps of trees and bamboo, mononuclear porphyrin or μ-oxygen-dinuclear metalloporphyrin catalyst, with strong basicity
Methanol is solvent, is passed through oxygen, and o-nitrobenzaldehyde crude product is obtained by the reaction at 25-60 DEG C, using conventional method separation, purification
Afterwards, o-nitrobenzaldehyde fine work is obtained.Under the catalyst amount of this method, reaction temperature and pressure are relatively low, therefore aoxidize deep
It spends easily controllable, the selectivity of oxidation product o-nitrobenzaldehyde can be improved.It is a kind of disclosed in Chinese patent CN 105439867A
The preparation method of o-nitrobenzaldehyde, by the double alkyl nitrile catalyst heating stirrings of ortho-methylnitrobenzene, halogenated aryl hydrocarbon solvent and azo
After bromine is added dropwise, be heated to reflux to bromine color fade, hydrogen peroxide reflux be added, o-nitrobenzyl bromide is obtained, then by adjacent nitre
Aqueous sodium carbonate is added in base benzyl bromide, is heated to reflux hydrolysis, obtains nitro alcohol target product and sodium bromide by-product
The nitro alcohol target product isolated is added in sodium hydroxide object, and agitation and dropping hydrogen peroxide, adds at 25-35 DEG C
Hot back flow reaction generates o-nitrobenzaldehyde.The preparation method reaction condition is mild, and high income reduces the life of organic by-products
At with inorganic salts (acid) discharge of wastewater, and the purity of the o-nitrobenzaldehyde prepared is high.By the above-mentioned prior art it is found that with adjacent nitre
It is difficult control in terms of controlling degree of oxidation that base toluene, which prepares o-nitrobenzaldehyde, and has intractable by-product and generate, no
Conducive to environmental protection.
Invention content
The technical problem to be solved in the present invention is to provide a kind of producers of the o-nitrobenzaldehyde based on potassium ethoxide/niobium
Method, in anhydrous conditions without hydrolysis, can obtain the neighbour insoluble in solvent using potassium ethoxide/niobium as condensation catalyst
Nitrobenzene ethyl pyruvate enol potassium/niobium salt, then through ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt oxidation reaction, be prepared into
To o-nitrobenzaldehyde.
In order to solve the above technical problems, the technical scheme is that：
A kind of production method of the o-nitrobenzaldehyde based on potassium ethoxide/niobium, includes the following steps：
(1) under nitrogen atmosphere, potassium being added in hexamethylene, the benzole soln of niobium chloride is added in supersonic oscillations processing,
Ethyl alcohol is added dropwise under cryogenic, continues supersonic oscillations, filters, removes benzene, obtains the cyclohexane solution of potassium ethoxide/niobium；
(2) ortho-methylnitrobenzene and diethy-aceto oxalate are added to the cyclohexane solution of potassium ethoxide/niobium prepared by step (1), room
Temperature stirring is complete to dissolving, and slow heating stirring to aneroid evacuator body, room temperature is down in stirring, and after being washed with hexamethylene, drying obtains
To ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt；
(3) under nitrogen light protected environment, ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt is slowly added to 30% mistake in batches
The in the mixed solvent of hydrogen oxide and hexamethylene is added dropwise a small amount of water, stirs at low ambient temperatures, filters layering, and vacuum drying obtains
O-nitrobenzaldehyde.
As a preferred embodiment of the above technical solution, the power that supersonic oscillations are handled in the step (1) is 250-500W, when
Between be 15-30min.
As a preferred embodiment of the above technical solution, the ratio of the amount of the substance of potassium and niobium is 2-3 in the step (1):1.
As a preferred embodiment of the above technical solution, the temperature of cryogenic conditions is 5-10 DEG C in the step (1), ethyl alcohol and potassium with
The ratio of the amount of the total substance of niobium is 1-2:1.
As a preferred embodiment of the above technical solution, ortho-methylnitrobenzene, diethy-aceto oxalate and potassium ethoxide/niobium in the step (2)
Substance amount ratio be 1:1.2-1.4:1.1-1.3.
As a preferred embodiment of the above technical solution, the heating rate of slow heating stirring is 5 DEG C/min in the step (2),
Heating temperature is 30-90 DEG C, stir speed (S.S.) 150-250r/min.
As a preferred embodiment of the above technical solution, in the step (3) ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt and
The ratio of the amount of the substance of 30% hydrogen peroxide is 1:2-2.5.
As a preferred embodiment of the above technical solution, the time being slowly added in batches in the step (3) is 10-20min.
As a preferred embodiment of the above technical solution, the condition stirred under low temperature environment in the step (3) is, first at 0-5 DEG C
Lower stirring is warming up to 10-15 DEG C, the reaction was continued 30-45min to after feeding with the rate of 0.5-1 DEG C/min.
As a preferred embodiment of the above technical solution, the dosage of water accounts for the 1-3% of total system in the step (3).
Compared with prior art, the invention has the advantages that：
(1) present invention uses potassium ethoxide/girl as condensation catalyst, and metal alkoxide activity is high, in anhydrous conditions,
Reaction will not be hydrolyzed, reaction can rest on condensation reaction, obtain the ortho-nitrophenyl ethyl pyruvate insoluble in organic solvent
Enol potassium/niobium salt solid, the present invention is using two kinds of metal alkoxides as condensation catalyst, catalytic activity higher, milder, and
Both potassium and girl are uniformly mixed in the potassium ethoxide/girl prepared using potassium and girl's salt, and purity is high, and activity is high, can further shorten
Reaction time improves the yield of condensation reaction, and ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt of preparation does not dissolve in hexamethylene,
It can easily separate.Then again that ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt solid is even in the low temperature of hydrogen peroxide
Reaction generates o-nitrobenzaldehyde under fast catalytic action, and oxidation reaction is mild, is not easy overreact, the high income of product, purity
It is high.
(2) preparation method of the invention is simple, and controllability is strong, and reaction condition is mild, at low cost, and ortho-methylnitrobenzene turns
Rate is high, and the by-product of preparation method is few, and business efficiency is good.
Specific implementation mode
Below in conjunction with specific embodiment, the present invention will be described in detail, herein illustrative examples and explanation of the invention
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1：
(1) under nitrogen atmosphere, potassium is added in hexamethylene, supersonic oscillations handle 15min under 250W power, press
Ratio according to the amount of potassium and the substance of niobium is 2:1, the benzole soln of niobium chloride is added, ethyl alcohol, wherein second are added dropwise under 5 DEG C of cryogenic conditions
Alcohol and the ratio of potassium and the amount of the total substance of niobium are 1:1, continue supersonic oscillations 15min, filter, removes benzene, obtain potassium ethoxide/niobium
Cyclohexane solution.
(2) it is 1 according to the ratio of the amount of the substance of ortho-methylnitrobenzene, diethy-aceto oxalate and potassium ethoxide/niobium:1.2:1.1, it will be adjacent
The cyclohexane solution of potassium ethoxide/niobium is added in nitrotoleune and diethy-aceto oxalate, is stirred at room temperature to dissolving completely, with 5 DEG C/min's
Rate is slowly heated to 30 DEG C, is stirred to aneroid evacuator body with the rate of 150r/min, stirring is down to room temperature, is washed with hexamethylene
Afterwards, it dries, obtains ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt.
(3) under nitrogen light protected environment, according to ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt and 30% hydrogen peroxide
The ratio of the amount of substance is 1:2, it is first at 0 DEG C, ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt is in batches slow in 10min
The in the mixed solvent of 30% hydrogen peroxide and hexamethylene is added, 1% water for accounting for total system is added dropwise, then with 0.5 DEG C/min's
Rate is warming up to 10 DEG C, the reaction was continued 30min, filters layering, and vacuum drying obtains o-nitrobenzaldehyde.
Embodiment 2：
(1) under nitrogen atmosphere, potassium is added in hexamethylene, supersonic oscillations handle 30min under 500W power, press
Ratio according to the amount of potassium and the substance of niobium is 3:1, the benzole soln of niobium chloride is added, ethyl alcohol is added dropwise under 10 DEG C of cryogenic conditions, wherein
Ethyl alcohol and the ratio of potassium and the amount of the total substance of niobium are 2:1, continue supersonic oscillations 30min, filter, remove benzene, obtain potassium ethoxide/
The cyclohexane solution of niobium.
(2) it is 1 according to the ratio of the amount of the substance of ortho-methylnitrobenzene, diethy-aceto oxalate and potassium ethoxide/niobium:1.4:1.3, it will be adjacent
The cyclohexane solution of potassium ethoxide/niobium is added in nitrotoleune and diethy-aceto oxalate, is stirred at room temperature to dissolving completely, with 5 DEG C/min's
Rate is slowly heated to 90 DEG C, is stirred to aneroid evacuator body with the rate of 250r/min, stirring is down to room temperature, is washed with hexamethylene
Afterwards, it dries, obtains ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt.
(3) under nitrogen light protected environment, according to ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt and 30% hydrogen peroxide
The ratio of the amount of substance is 1:2.5, first at 5 DEG C, ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt is delayed in batches in 20min
The slow in the mixed solvent that 30% hydrogen peroxide and hexamethylene is added, is added dropwise 3% water for accounting for total system, then with 1 DEG C/min's
Rate is warming up to 15 DEG C, the reaction was continued 45min, filters layering, and vacuum drying obtains o-nitrobenzaldehyde.
Embodiment 3：
(1) under nitrogen atmosphere, potassium is added in hexamethylene, supersonic oscillations handle 20min under 300W power, press
Ratio according to the amount of potassium and the substance of niobium is 2.5:1, the benzole soln of niobium chloride is added, ethyl alcohol is added dropwise under 7 DEG C of cryogenic conditions, wherein
Ethyl alcohol and the ratio of potassium and the amount of the total substance of niobium are 1.4:1, continue supersonic oscillations 20min, filter, removes benzene, obtain ethyl alcohol
The cyclohexane solution of potassium/niobium.
(2) it is 1 according to the ratio of the amount of the substance of ortho-methylnitrobenzene, diethy-aceto oxalate and potassium ethoxide/niobium:1.2:1.1, it will be adjacent
The cyclohexane solution of potassium ethoxide/niobium is added in nitrotoleune and diethy-aceto oxalate, is stirred at room temperature to dissolving completely, with 5 DEG C/min's
Rate is slowly heated to 60 DEG C, is stirred to aneroid evacuator body with the rate of 200r/min, stirring is down to room temperature, is washed with hexamethylene
Afterwards, it dries, obtains ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt.
(3) under nitrogen light protected environment, according to ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt and 30% hydrogen peroxide
The ratio of the amount of substance is 1:2.3, first at 3 DEG C, ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt is delayed in batches in 15min
The slow in the mixed solvent that 30% hydrogen peroxide and hexamethylene is added, is added dropwise 2% water for accounting for total system, then with 0.8 DEG C/min
Rate be warming up to 14 DEG C, the reaction was continued 35min filters layering, and vacuum drying obtains o-nitrobenzaldehyde.
Embodiment 4：
(1) under nitrogen atmosphere, potassium is added in hexamethylene, supersonic oscillations handle 25min under 450W power, press
Ratio according to the amount of potassium and the substance of niobium is 2.7:1, the benzole soln of niobium chloride is added, ethyl alcohol is added dropwise under 7 DEG C of cryogenic conditions, wherein
Ethyl alcohol and the ratio of potassium and the amount of the total substance of niobium are 1.4:1, continue supersonic oscillations 25min, filter, removes benzene, obtain ethyl alcohol
The cyclohexane solution of potassium/niobium.
(2) it is 1 according to the ratio of the amount of the substance of ortho-methylnitrobenzene, diethy-aceto oxalate and potassium ethoxide/niobium:1.2:1.2, it will be adjacent
The cyclohexane solution of potassium ethoxide/niobium is added in nitrotoleune and diethy-aceto oxalate, is stirred at room temperature to dissolving completely, with 5 DEG C/min's
Rate is slowly heated to 80 DEG C, is stirred to aneroid evacuator body with the rate of 180r/min, stirring is down to room temperature, is washed with hexamethylene
Afterwards, it dries, obtains ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt.
(3) under nitrogen light protected environment, according to ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt and 30% hydrogen peroxide
The ratio of the amount of substance is 1:2.3, first at 1 DEG C, ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt is delayed in batches in 17min
The slow in the mixed solvent that 30% hydrogen peroxide and hexamethylene is added, is added dropwise 2.5% water for accounting for total system, then with 0.8 DEG C/
The rate of min is warming up to 14 DEG C, the reaction was continued 40min, filters layering, and vacuum drying obtains o-nitrobenzaldehyde.
Embodiment 5：
(1) under nitrogen atmosphere, potassium is added in hexamethylene, supersonic oscillations handle 20min under 360W power, press
Ratio according to the amount of potassium and the substance of niobium is 2.3:1, the benzole soln of niobium chloride is added, ethyl alcohol is added dropwise under 8 DEG C of cryogenic conditions, wherein
Ethyl alcohol and the ratio of potassium and the amount of the total substance of niobium are 1.3:1, continue supersonic oscillations 25min, filter, removes benzene, obtain ethyl alcohol
The cyclohexane solution of potassium/niobium.
(2) it is 1 according to the ratio of the amount of the substance of ortho-methylnitrobenzene, diethy-aceto oxalate and potassium ethoxide/niobium:1.4:1.1, it will be adjacent
The cyclohexane solution of potassium ethoxide/niobium is added in nitrotoleune and diethy-aceto oxalate, is stirred at room temperature to dissolving completely, with 5 DEG C/min's
Rate is slowly heated to 50 DEG C, is stirred to aneroid evacuator body with the rate of 200r/min, stirring is down to room temperature, is washed with hexamethylene
Afterwards, it dries, obtains ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt.
(3) under nitrogen light protected environment, according to ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt and 30% hydrogen peroxide
The ratio of the amount of substance is 1:2.2, first at 3 DEG C, ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt is delayed in batches in 13min
The slow in the mixed solvent that 30% hydrogen peroxide and hexamethylene is added, is added dropwise 2% water for accounting for total system, then with 0.9 DEG C/min
Rate be warming up to 14 DEG C, the reaction was continued 35min filters layering, and vacuum drying obtains o-nitrobenzaldehyde.
Embodiment 6：
(1) under nitrogen atmosphere, potassium is added in hexamethylene, supersonic oscillations handle 30min under 250W power, press
Ratio according to the amount of potassium and the substance of niobium is 2:1, the benzole soln of niobium chloride is added, ethyl alcohol is added dropwise under 10 DEG C of cryogenic conditions, wherein
Ethyl alcohol and the ratio of potassium and the amount of the total substance of niobium are 1:1, continue supersonic oscillations 30min, filter, remove benzene, obtain potassium ethoxide/
The cyclohexane solution of niobium.
(2) it is 1 according to the ratio of the amount of the substance of ortho-methylnitrobenzene, diethy-aceto oxalate and potassium ethoxide/niobium:1.2:1.3, it will be adjacent
The cyclohexane solution of potassium ethoxide/niobium is added in nitrotoleune and diethy-aceto oxalate, is stirred at room temperature to dissolving completely, with 5 DEG C/min's
Rate is slowly heated to 30 DEG C, is stirred to aneroid evacuator body with the rate of 250r/min, stirring is down to room temperature, is washed with hexamethylene
Afterwards, it dries, obtains ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt.
(3) under nitrogen light protected environment, according to ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt and 30% hydrogen peroxide
The ratio of the amount of substance is 1:2, it is first at 5 DEG C, ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt is in batches slow in 10min
The in the mixed solvent of 30% hydrogen peroxide and hexamethylene is added, 3% water for accounting for total system is added dropwise, then with 0.5 DEG C/min's
Rate is warming up to 15 DEG C, the reaction was continued 30min, filters layering, and vacuum drying obtains o-nitrobenzaldehyde.
After testing, the yield for the o-nitrobenzaldehyde that prepared by embodiment 1-6 and the result of purity are as follows：
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | |
| Yield (%) | 54.2 | 56.7 | 55.1 | 54.7 | 55.0 | 55.8 |
| Purity (%) | 98.7 | 99.4 | 99.0 | 98.8 | 99.0 | 99.1 |
As seen from the above table, under conditions of the present invention prepares reaction condition milder, the receipts of the o-nitrobenzaldehyde of preparation
Rate and purity significantly improve.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology can all carry out modifications and changes to above-described embodiment without violating the spirit and scope of the present invention.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should by the present invention claim be covered.
Claims (10)
1. a kind of production method of the o-nitrobenzaldehyde based on potassium ethoxide/niobium, which is characterized in that include the following steps：
(1) under nitrogen atmosphere, potassium is added in hexamethylene, the benzole soln of niobium chloride is added, low in supersonic oscillations processing
Ethyl alcohol is added dropwise under the conditions of temperature, continues supersonic oscillations, filters, removes benzene, obtains the cyclohexane solution of potassium ethoxide/niobium；
(2) ortho-methylnitrobenzene and diethy-aceto oxalate are added to the cyclohexane solution of potassium ethoxide/niobium prepared by step (1), room temperature is stirred
It mixes to dissolving completely, slow heating stirring to aneroid evacuator body, room temperature is down in stirring, and after being washed with hexamethylene, drying obtains neighbour
Nitrobenzene ethyl pyruvate enol potassium/niobium salt；
(3) under nitrogen light protected environment, ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt is slowly added to 30% peroxidating in batches
The in the mixed solvent of hydrogen and hexamethylene is added dropwise a small amount of water, stirs at low ambient temperatures, filters layering, and vacuum drying obtains adjacent nitre
Benzaldehyde.
2. a kind of production method of o-nitrobenzaldehyde based on potassium ethoxide/niobium according to claim 1, feature exist
In：The power that supersonic oscillations are handled in the step (1) is 250-500W, time 15-30min.
3. a kind of production method of o-nitrobenzaldehyde based on potassium ethoxide/niobium according to claim 1, feature exist
In：The ratio of the amount of the substance of potassium and niobium is 2-3 in the step (1):1.
4. a kind of production method of o-nitrobenzaldehyde based on potassium ethoxide/niobium according to claim 1, feature exist
In：The temperature of cryogenic conditions is 5-10 DEG C in the step (1), and ethyl alcohol and the ratio of potassium and the amount of the total substance of niobium are 1-2:1.
5. a kind of production method of o-nitrobenzaldehyde based on potassium ethoxide/niobium according to claim 1, feature exist
In：The ratio of the amount of the substance of ortho-methylnitrobenzene, diethy-aceto oxalate and potassium ethoxide/niobium is 1 in the step (2):1.2-1.4:
1.1-1.3。
6. a kind of production method of o-nitrobenzaldehyde based on potassium ethoxide/niobium according to claim 1, feature exist
In：The heating rate of slow heating stirring is 5 DEG C/min in the step (2), and heating temperature is 30-90 DEG C, and stir speed (S.S.) is
150-250r/min。
7. a kind of production method of o-nitrobenzaldehyde based on potassium ethoxide/niobium according to claim 1, feature exist
In：The ratio of the amount of the substance of ortho-nitrophenyl ethyl pyruvate enol potassium/niobium salt and 30% hydrogen peroxide is 1 in the step (3):
2-2.5。
8. a kind of production method of o-nitrobenzaldehyde based on potassium ethoxide/niobium according to claim 1, feature exist
In：The time being slowly added in batches in the step (3) is 10-20min.
9. a kind of production method of o-nitrobenzaldehyde based on potassium ethoxide/niobium according to claim 1, feature exist
In：The condition stirred under low temperature environment in the step (3) is, first at 0-5 DEG C stirring to after charging, with 0.5-1 DEG C/
The rate of min is warming up to 10-15 DEG C, the reaction was continued 30-45min.
10. a kind of production method of o-nitrobenzaldehyde based on potassium ethoxide/niobium according to claim 1, feature exist
In：The dosage of water accounts for the 1-3% of total system in the step (3).
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| CN1111232A (en) * | 1994-05-03 | 1995-11-08 | 中国石油化工总公司上海石油化工研究院 | Preparation of ortho-nitrobenzaldehyde from ortho-nitrophenyl-pyruvic acid |
| CN104418753A (en) * | 2013-08-21 | 2015-03-18 | 南京理工大学 | Method for green-catalytically synthesizing nitrobenzaldehyde |
| CN105439867A (en) * | 2014-08-22 | 2016-03-30 | 南京理工大学 | A preparing method of 2-nitrobenzaldehyde |
| CN105622483A (en) * | 2016-03-01 | 2016-06-01 | 苏州艾缇克药物化学有限公司 | Synthesis method of 4-nitroindole |
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