CN104447246B - Method for preparing o-methoxybenzaldehyde by using micro-reaction device - Google Patents
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 55
- PKZJLOCLABXVMC-UHFFFAOYSA-N 2-Methoxybenzaldehyde Chemical compound COC1=CC=CC=C1C=O PKZJLOCLABXVMC-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 19
- VAYGXNSJCAHWJZ-UHFFFAOYSA-N dimethyl sulfate Chemical compound COS(=O)(=O)OC VAYGXNSJCAHWJZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- 239000003513 alkali Substances 0.000 claims abstract description 3
- 239000012043 crude product Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 41
- 239000000243 solution Substances 0.000 claims description 13
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims 1
- 150000007984 tetrahydrofuranes Chemical group 0.000 claims 1
- 239000006227 byproduct Substances 0.000 abstract description 2
- 239000012456 homogeneous solution Substances 0.000 abstract 2
- SMQUZDBALVYZAC-UHFFFAOYSA-N salicylaldehyde Chemical compound OC1=CC=CC=C1C=O SMQUZDBALVYZAC-UHFFFAOYSA-N 0.000 abstract 2
- 230000003321 amplification Effects 0.000 abstract 1
- 238000003199 nucleic acid amplification method Methods 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 16
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 15
- 239000000047 product Substances 0.000 description 12
- 241000196324 Embryophyta Species 0.000 description 6
- 239000012530 fluid Substances 0.000 description 6
- 208000035126 Facies Diseases 0.000 description 5
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 5
- 239000000376 reactant Substances 0.000 description 5
- 238000004064 recycling Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 239000001117 sulphuric acid Substances 0.000 description 5
- 235000011149 sulphuric acid Nutrition 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical group C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 3
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical class COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 description 3
- 150000004702 methyl esters Chemical class 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 150000001299 aldehydes Chemical class 0.000 description 2
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- OJURWUUOVGOHJZ-UHFFFAOYSA-N methyl 2-[(2-acetyloxyphenyl)methyl-[2-[(2-acetyloxyphenyl)methyl-(2-methoxy-2-oxoethyl)amino]ethyl]amino]acetate Chemical compound C=1C=CC=C(OC(C)=O)C=1CN(CC(=O)OC)CCN(CC(=O)OC)CC1=CC=CC=C1OC(C)=O OJURWUUOVGOHJZ-UHFFFAOYSA-N 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- ZRSNZINYAWTAHE-UHFFFAOYSA-N p-methoxybenzaldehyde Chemical compound COC1=CC=C(C=O)C=C1 ZRSNZINYAWTAHE-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 235000013599 spices Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- DTFKRVXLBCAIOZ-UHFFFAOYSA-N 2-methylanisole Chemical compound COC1=CC=CC=C1C DTFKRVXLBCAIOZ-UHFFFAOYSA-N 0.000 description 1
- RGHHSNMVTDWUBI-UHFFFAOYSA-N 4-hydroxybenzaldehyde Chemical compound OC1=CC=C(C=O)C=C1 RGHHSNMVTDWUBI-UHFFFAOYSA-N 0.000 description 1
- 244000020998 Acacia farnesiana Species 0.000 description 1
- 235000003074 Acacia farnesiana Nutrition 0.000 description 1
- 241001672694 Citrus reticulata Species 0.000 description 1
- 244000020551 Helianthus annuus Species 0.000 description 1
- 235000003222 Helianthus annuus Nutrition 0.000 description 1
- 241000333181 Osmanthus Species 0.000 description 1
- 235000019082 Osmanthus Nutrition 0.000 description 1
- 241000775848 Syringa oblata Species 0.000 description 1
- 244000290333 Vanilla fragrans Species 0.000 description 1
- 235000009499 Vanilla fragrans Nutrition 0.000 description 1
- 235000012036 Vanilla tahitensis Nutrition 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229960000723 ampicillin Drugs 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 229940124623 antihistamine drug Drugs 0.000 description 1
- 239000000739 antihistaminic agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- -1 hydroxyl Ampicillin Chemical compound 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 1
- 239000005445 natural material Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/61—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups
- C07C45/64—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by introduction of functional groups containing oxygen only in singly bound form
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for preparing o-methoxybenzaldehyde by a micro-reaction device, which comprises the following steps: dissolving salicylaldehyde in a strong alkali water solution to obtain a homogeneous solution; dissolving dimethyl sulfate in an organic solvent to obtain a homogeneous solution; respectively and simultaneously pumping the two homogeneous phase solutions into a micro-reaction device, wherein the reaction temperature is 70-120 ℃, and the reaction residence time is 1-10 min; collecting the effluent liquid, namely the o-methoxybenzaldehyde crude product. The micro-reactor has the advantages of large specific surface area, high transfer rate, short contact time, few by-products and very strong heat transfer and mass transfer capacities; rapid and direct amplification, high safety, good operability and the like.
Description
Technical field
The invention belongs to chemosynthesis technical field, be specifically related to one and utilize micro-reaction device to prepare o-methoxybenzaldehyde
Method.
Background technology
O-methoxybenzaldehyde, also known as Fructus Foeniculi aldehyde, is a kind of organic synthesis intermediate, for medicine, food and dailyization
Learn industry.Be widely used in the spice of preparation floral type as middle taste type spice, it has lasting Fructus Crataegi fragrance, Fructus Crataegi
Flower, sunflower, Syringa oblata Lindl. essence do main body fragrant material；Dressing agent is made in osmanthus flower fragrance；Can also be used for daily essence and
Food flavor, coordinates with the quintessence oil of mandarin orange etc., and effect is fine.Medical industry is used for manufacture antimicrobial medicine hydroxyl
Ampicillin etc., are the intermediate of antihistamine drug.As the excellent brightener of non-cyanogen galvanization DE additive, can be
Anode polarization is improved, it is thus achieved that bright coating in wider current density range.
The preparation of o-methoxybenzaldehyde has many methods.1. plant extraction method: Fructus Foeniculi aldehyde is present in Oleum Anisi Stellati, transplants
In the natural material such as trailing plants oil, Acacia farnesiana Willd. caul-fat, vanilla extractum, some oxidants can be added and distintegrant extracts greatly
Anisaldehyde.But this complex process, yield is low, is the most eliminated；2. chemical synthesis: different according to raw material sources,
There is kinds of processes route, as orthoresol method, methyl phenyl ethers anisole method, O-methoxy toluene oxidation method, hydroxy benzaldehyde methylate
Methods etc., each method has its pluses and minuses.
Microreactor be a kind of by means of special micro-processing with solid matrix manufacture can be used for carry out chemical reaction
Three dimensional structure element.Microreactor usually contains little channel size (equivalent diameter is less than 500 μm) and passage is various
Property, fluid flows in these passages, and require in these passages occur required by reaction.Which results in
The chemical device of micro-structure has the biggest surface area/volume ratio rate.G.WieBmeier et al. is in micro-reacting tcchnology state
The micro passage reaction for heterogeneous catalytic reaction is described in the meeting of border.
Summary of the invention
The technical problem to be solved is to provide and a kind of efficient, free of contamination utilizes the adjacent methoxy of micro-reaction device preparation
The method of benzaldehyde.
For solving above-mentioned technical problem, the technical solution used in the present invention is as follows:
A kind of micro-reaction device prepares the method for o-methoxybenzaldehyde, and it comprises the steps:
(1) salicylide is dissolved in strong alkali aqueous solution, obtains homogeneous phase solution；
(2) dimethyl sulfate is dissolved in organic solvent, obtains homogeneous phase solution；
(3) the both of which phase solution that step (1) and step (2) obtain is pumped in micro-reaction device the most simultaneously,
Reaction temperature is 70～120 DEG C, and reaction time is 1～10min；
(4) collect trickle, be o-methoxybenzaldehyde crude product.
In step (1), described highly basic is sodium hydroxide or potassium hydroxide.
In step (1), in the homogeneous phase solution obtained, the concentration of salicylide is 0.1～0.2g/ml, salicylide and highly basic
Mol ratio is 1:1.0～1.2.
In step (2), described organic solvent is oxolane, dimethylformamide, Isosorbide-5-Nitrae-dioxane or spreads out for it
Raw kind solvent.
In step (2), in the homogeneous phase solution obtained, the concentration of dimethyl sulfate is 0.1～0.3g/ml.
In step (3), described micro-reaction device is by the liquor inlet being linked in sequence by connecting tube, T-shaped mixing valve
Door, micro passage reaction and material liquid outlet.
Wherein, a diameter of the 0.8 of described connecting tube～2mm.
Wherein, described micro passage reaction volume is 2～10ml.
In step (3), salicylide controls at 1:1.0～1.5 with the reaction mol ratio of dimethyl sulfate.
In step (3), both of which phase solution flow rate is 0.1～5ml/min.
In step (3), reaction temperature is preferably 70～100 DEG C, and reaction time is 1～10min.
Beneficial effect: it is big that microreactor has specific surface area, transfer rate is high, and time of contact is short, and by-product is few, heat transfer,
Mass transfer ability is the strongest；Quickly, directly amplify, the features such as safety is high, good operability；Micro-response system is in module
The parallel system of structure, has good portability feature, may be implemented in product and makes land used dispersion build and be produced in situ in, supply,
Really realize chemical plant portability, and production can be regulated according to market situation increase and decrease port number and replacing module, have
The highest operating flexibility.The o-methoxybenzaldehyde production method technique that the present invention provides is simple, can produce continuously, has
Higher processing safety and higher selectivity, reaction volume is little, the time is short less to equipment corrosion；Topmost
Being to overcome dimethyl sulfate the person injures the pollution to environment, operation full safety is closed.Meanwhile, micro-leading to is utilized
The High Efficiency Thermal mass transfer ability of road reactor and be prone to the feature directly amplified, converts rate a height of more than 85%, product matter
Measure, energy consumption low, be a kind of environmental protection method of synthesizing o-methoxybenzaldehyde efficiently.
Accompanying drawing explanation
Fig. 1 is the structural representation of micro passage reaction of the present invention.
Fig. 2 is the reaction equation of the present invention.
Detailed description of the invention
According to following embodiment, the present invention be may be better understood.But, as it will be easily appreciated by one skilled in the art that reality
Execute the content described by example and be merely to illustrate the present invention, and should be also without limitation on not described in detail in claims
The present invention.
Following microchannel reaction unit is by the liquor inlet being linked in sequence by connecting tube, T-shaped mixing valve, microchannel plate
Answering device and material liquid outlet, concrete assembling sees that Fig. 1, two of which reaction raw materials storage tank connect respective feed liquid by connecting tube
Import is connected with T-shaped mixing valve the most respectively, and this connecting tube is respectively equipped with pump, T-shaped mixing valve by connecting tube with
Micro passage reaction connects, and micro passage reaction is connected with material liquid outlet by connecting tube, and described head tank is 250ml
Conical flask, micro passage reaction model is vapourtac R series, is purchased from De Xiang International Technology company.Experiment is used
The reagent arrived is all AR, is purchased from Shanghai Ling Feng chemical reagent company limited.
Embodiment 1:
In the reaction unit of microchannel, connecting tube diameter is 0.8mm, and a length of 15cm of feed tube, T-valve Men Yuwei are logical
The a length of 32cm of connecting tube between road reactor, a length of 32cm of connecting tube between microreactor and outlet；Micro-logical
Road reactor volume is 5ml.
Take salicylide 0.025mol (3.05g), join and the aqueous solution containing 0.025mol sodium hydroxide stirs in homogeneously,
Obtain mixeding liquid volume 30mL；Weigh 0.025mol (3.15g) dimethyl sulfate, add THF and be diluted to 30mL.By two
Plant material to be entered in micro passage reaction by T-valve door mixing pump.Two kinds of reactant liquor fluids flow through with 2.5mL/min respectively
Microreactor, salicylide is 1:1.0 with the reaction mol ratio of dimethyl sulfate, and temperature of reactor is 110 DEG C, and reaction stops
Time is 1min, and thick product is collected in outlet；Excessive sodium hydrate is added to have hydrolyzed the sulphuric acid two of residual in thick product
Methyl ester, is stirred overnight.It is extracted with ethyl acetate three times, recycling 1mol/L sodium hydrate aqueous solution washing organic facies,
Adding anhydrous magnesium sulfate to be dried, rotation is evaporated dry.Productivity is 90.2%.
Embodiment 2:
In the reaction unit of microchannel, connecting tube diameter is 2.0mm, and a length of 15cm of feed tube, T-valve Men Yuwei are logical
The a length of 32cm of connecting tube between road reactor, a length of 32cm of connecting tube between microreactor and outlet；Micro-logical
Road reactor volume is 2ml.
Take salicylide 0.025mol (3.05g), join and the aqueous solution containing 0.0275mol sodium hydroxide stirs in homogeneously,
Obtain mixeding liquid volume 30mL；Weigh 0.0275mol (3.47g) dimethyl sulfate, add DMF and be diluted to 30mL.Will
Two kinds of materials are entered in micro passage reaction by T-valve door mixing pump.Two kinds of reactant liquor fluids flow with 0.1mL/min respectively
Through microreactor, it is 1:1.1 that salicylide and dimethyl sulfate react mol ratio, and temperature of reactor is 90 DEG C, and reaction stops
Time is 10min, and thick product is collected in outlet；Excessive sodium hydrate is added to have hydrolyzed the sulphuric acid two of residual in thick product
Methyl ester, is stirred overnight.It is extracted with ethyl acetate three times, recycling 1mol/L sodium hydrate aqueous solution washing organic facies,
Adding anhydrous magnesium sulfate to be dried, rotation is evaporated dry.Productivity is 88.6%.
Embodiment 3:
In the reaction unit of microchannel, connecting tube diameter is 1.0mm, and a length of 15cm of feed tube, T-valve Men Yuwei are logical
The a length of 32cm of connecting tube between road reactor, a length of 32cm of connecting tube between microreactor and outlet；Micro-logical
Road reactor volume is 10ml.
Take salicylide 0.05mol (6.05g), join and the aqueous solution containing 0.0525mol sodium hydroxide stirs in homogeneously,
Obtain mixeding liquid volume 40mL；Weigh 0.065mol (8.19g) dimethyl sulfate, add dioxane and be diluted to 40mL.Will
Two kinds of materials are entered in micro passage reaction by T-valve door mixing pump.Two kinds of reactant liquor fluids flow with 2.5mL/min respectively
Through microreactor, salicylide is 1:1.3 with the reaction mol ratio of dimethyl sulfate, and temperature of reactor is 70 DEG C, and reaction stops
Staying the time is 2min, and thick product is collected in outlet；Excessive sodium hydrate is added to have hydrolyzed the sulphuric acid of residual in thick product
Dimethyl ester, is stirred overnight.It is extracted with ethyl acetate three times, recycling 1mol/L sodium hydrate aqueous solution washing organic facies,
Adding anhydrous magnesium sulfate to be dried, rotation is evaporated dry.Productivity is 95.6%.
Embodiment 4:
In the reaction unit of microchannel, connecting tube diameter is 1.0mm, and a length of 15cm of feed tube, T-valve Men Yuwei are logical
The a length of 32cm of connecting tube between road reactor, a length of 32cm of connecting tube between microreactor and outlet；Micro-logical
Road reactor volume is 5ml.
Take salicylide 0.05mol (6.05g), join and the aqueous solution containing 0.055mol sodium hydroxide stirs in homogeneously,
Obtain mixeding liquid volume 40mL；Weigh 0.06mol (7.56g) dimethyl sulfate, add DMF and be diluted to 40mL.By two
Plant material to be entered in micro passage reaction by T-valve door mixing pump.Two kinds of reactant liquor fluids flow through with 2.5mL/min respectively
Microreactor, salicylide is 1:1.2 with the reaction mol ratio of dimethyl sulfate, and temperature of reactor is 120 DEG C, and reaction stops
Time is 1min, and thick product is collected in outlet；Excessive sodium hydrate is added to have hydrolyzed the sulphuric acid two of residual in thick product
Methyl ester, is stirred overnight.It is extracted with ethyl acetate three times, recycling 1mol/L sodium hydrate aqueous solution washing organic facies,
Adding anhydrous magnesium sulfate to be dried, rotation is evaporated dry.Productivity is 91.6%.
Embodiment 5:
In the reaction unit of microchannel, connecting tube diameter is 1.2mm, and a length of 15cm of feed tube, T-valve Men Yuwei are logical
The a length of 32cm of connecting tube between road reactor, a length of 32cm of connecting tube between microreactor and outlet；Micro-logical
Road reactor volume is 5ml.
Take salicylide 0.05mol (6.05g), join and the aqueous solution containing 0.0525mol sodium hydroxide stirs in homogeneously,
Obtain mixeding liquid volume 32mL；Weigh 0.065mol (8.19g) dimethyl sulfate, add DMF and be diluted to 32mL.By two
Plant material to be entered in micro passage reaction by T-valve door mixing pump.Two kinds of reactant liquor fluids flow with 1.25mL/min respectively
Through microreactor, salicylide is 1:1.3 with the reaction mol ratio of dimethyl sulfate, and temperature of reactor is 70 DEG C, and reaction stops
Staying the time is 2min, and thick product is collected in outlet；Excessive sodium hydrate is added to have hydrolyzed the sulphuric acid of residual in thick product
Dimethyl ester, is stirred overnight.It is extracted with ethyl acetate three times, recycling 1mol/L sodium hydrate aqueous solution washing organic facies,
Adding anhydrous magnesium sulfate to be dried, rotation is evaporated dry.Productivity is 92.6%.
Claims (3)
1. the method that a micro-reaction device prepares o-methoxybenzaldehyde, it is characterised in that it comprises the steps:
(1) salicylide is dissolved in strong alkali aqueous solution, obtains homogeneous phase solution；
(2) dimethyl sulfate is dissolved in organic solvent, obtains homogeneous phase solution；
(3) the both of which phase solution that step (1) and step (2) obtain is pumped in micro-reaction device the most simultaneously,
Reaction temperature is 70～120 DEG C, and reaction time is 1～10min；
(4) collect trickle, be o-methoxybenzaldehyde crude product；
In step (1), described highly basic is sodium hydroxide or potassium hydroxide；
In step (1), in the homogeneous phase solution obtained, the concentration of salicylide is 0.1～0.2g/ml, salicylide and highly basic
Mol ratio is 1:1.0～1.2；
In step (2), described organic solvent is oxolane, dimethylformamide or Isosorbide-5-Nitrae-dioxane；
In step (2), in the homogeneous phase solution obtained, the concentration of dimethyl sulfate is 0.1～0.3g/ml；
In step (3), described micro-reaction device is by the liquor inlet being linked in sequence by connecting tube, T-shaped mixing valve
Door, micro passage reaction and material liquid outlet composition；Described micro passage reaction volume is 2～10ml；
In step (3), salicylide controls at 1:1.0～1.5 with the reaction mol ratio of dimethyl sulfate.
Micro-reaction device the most according to claim 1 prepares the method for o-methoxybenzaldehyde, it is characterised in that
A diameter of the 0.8 of described connecting tube～2mm.
Micro-reaction device the most according to claim 1 prepares the method for o-methoxybenzaldehyde, it is characterised in that
In step (3), both of which phase solution flow rate is 0.1～5ml/min.
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| CN106866453B (en) * | 2017-01-23 | 2019-03-22 | 齐鲁天和惠世制药有限公司 | A kind of method that microreactor prepares scheme for lacosamide |
| CN106866380B (en) * | 2017-02-20 | 2020-04-07 | 河北工业大学 | Method and equipment for preparing 2, 6-di-tert-butyl-p-cresol by using micro-reaction rectifying plate |
| CN108017524B (en) * | 2017-11-24 | 2021-03-12 | 天津大学 | Preparation method of 3, 4, 5-trimethoxybenzaldehyde |
| CN109264744A (en) * | 2018-10-19 | 2019-01-25 | 湖南雅城新材料有限公司 | A kind of recovery method as resource of low cost ferric phosphate nitrogen-containing wastewater |
| CN109482119B (en) * | 2018-12-12 | 2021-05-07 | 西南大学 | Nano molecular sieve microreactor for efficiently producing benzaldehyde and preparation method thereof |
| CN110256217B (en) * | 2019-04-29 | 2020-08-04 | 武汉理工大学 | Preparation method of o-methoxybenzaldehyde |
| CN111302915B (en) * | 2020-03-05 | 2022-06-17 | 复旦大学 | Method for preparing anisaldehyde through micro-channel continuous ozone oxidation |
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