CN113402451A - Preparation method of 2, 5-dibromopyridine - Google Patents
Preparation method of 2, 5-dibromopyridine Download PDFInfo
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- CN113402451A CN113402451A CN202110753552.XA CN202110753552A CN113402451A CN 113402451 A CN113402451 A CN 113402451A CN 202110753552 A CN202110753552 A CN 202110753552A CN 113402451 A CN113402451 A CN 113402451A
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- acetone
- bromosuccinimide
- dibromopyridine
- bromopyridine
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- ZHXUWDPHUQHFOV-UHFFFAOYSA-N 2,5-dibromopyridine Chemical compound BrC1=CC=C(Br)N=C1 ZHXUWDPHUQHFOV-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- PCLIMKBDDGJMGD-UHFFFAOYSA-N N-bromosuccinimide Chemical compound BrN1C(=O)CCC1=O PCLIMKBDDGJMGD-UHFFFAOYSA-N 0.000 claims abstract description 84
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 78
- ICSNLGPSRYBMBD-UHFFFAOYSA-N 2-aminopyridine Chemical compound NC1=CC=CC=N1 ICSNLGPSRYBMBD-UHFFFAOYSA-N 0.000 claims abstract description 54
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- WGOLHUGPTDEKCF-UHFFFAOYSA-N 5-bromopyridin-2-amine Chemical compound NC1=CC=C(Br)C=N1 WGOLHUGPTDEKCF-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 23
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims abstract description 22
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052794 bromium Inorganic materials 0.000 claims abstract description 22
- 239000007787 solid Substances 0.000 claims abstract description 22
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 229910021589 Copper(I) bromide Inorganic materials 0.000 claims description 10
- NKNDPYCGAZPOFS-UHFFFAOYSA-M copper(i) bromide Chemical compound Br[Cu] NKNDPYCGAZPOFS-UHFFFAOYSA-M 0.000 claims description 10
- 235000010288 sodium nitrite Nutrition 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 5
- 238000004821 distillation Methods 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 239000002994 raw material Substances 0.000 abstract description 9
- SLMHHOVQRSSRCV-UHFFFAOYSA-N 2,3-dibromopyridine Chemical compound BrC1=CC=CN=C1Br SLMHHOVQRSSRCV-UHFFFAOYSA-N 0.000 abstract description 2
- 238000001953 recrystallisation Methods 0.000 description 7
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 150000003222 pyridines Chemical class 0.000 description 3
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical group C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical group 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 239000002220 antihypertensive agent Substances 0.000 description 1
- 229940127088 antihypertensive drug Drugs 0.000 description 1
- 239000002246 antineoplastic agent Substances 0.000 description 1
- 229940041181 antineoplastic drug Drugs 0.000 description 1
- 239000003699 antiulcer agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000002085 irritant Substances 0.000 description 1
- 231100000021 irritant Toxicity 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/61—Halogen atoms or nitro radicals
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pyridine Compounds (AREA)
Abstract
The invention relates to the technical field of dibromopyridine preparation, and discloses a preparation method of 2, 5-dibromopyridine, which comprises the following steps of S1: mixing and reacting, namely putting 2-aminopyridine into a reactor, then adding acetone, and then adding a bromization reagent bromine and N-bromosuccinimide; s2: recovering acetone, distilling under reduced pressure to recover acetone, filtering, and collecting the residual solid; s3: and (3) preparing a finished product, namely putting the collected residual solid into a reactor, then adding a sodium hydroxide solution, stirring and mixing, and filtering after mixing to obtain the 2-amino-5-bromopyridine. According to the invention, the reaction efficiency of the N-bromosuccinimide can be improved, the using amount of the N-bromosuccinimide is reduced, the cost is reduced by adding the N-bromosuccinimide in batches and heating, the raw materials can be recycled by the step of recovering the acetone, the cost is reduced, and the yield and the purity of the 2-amino-5-bromopyridine can be improved.
Description
Technical Field
The invention relates to the technical field of dibromopyridine preparation, and particularly relates to a preparation method of 2, 5-dibromopyridine.
Background
2, 5-dibromopyridine is an organic chemical substance, has a chemical formula of C5H3Br2N, is also a high molecular chemical raw material, is white to light yellow crystalline powder, has a melting point of 93-95 ℃, is soluble in water, is slightly soluble in benzene and alcohol, and is toxic and irritant; the pyridine derivatives are widely used in the synthesis of pesticides, medicines and natural products, such as antibiotics, anti-tumor drugs, anti-ulcer drugs, antihypertensive drugs and the like, pyridine rings and benzene rings are bioisosteres, and the pyridine rings have higher biological activity and smaller toxic and side effects.
Pyridine derivatives are general potential basic units of nitrogen-containing bioactive molecules, alkaloids contain saturated six-membered nitrogen heterocyclic structures, so that alkaloid skeleton units can be skillfully constructed through the pyridine derivatives, and the method has important significance for synthesis of nitrogen-containing heterocyclic alkaloids.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a preparation method of 2, 5-dibromopyridine, and solves the problems that the existing synthesis method of 2, 5-dibromopyridine has high cost and low efficiency and can not meet the requirements of people.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of 2, 5-dibromopyridine comprises the following steps:
s1: mixing and reacting, namely putting 2-aminopyridine into a reactor, then adding acetone, and then adding a bromization reagent bromine and N-bromosuccinimide;
s2: recovering acetone, distilling under reduced pressure to recover acetone, filtering, and collecting the residual solid;
s3: preparing a finished product, namely putting the collected residual solid into a reactor, adding a sodium hydroxide solution, stirring and mixing, and filtering after mixing to obtain 2-amino-5-bromopyridine;
s4: drying, namely drying the obtained 2-amino-5-bromopyridine, and then collecting;
s5: catalyzing, adding 2-amino-5-bromopyridine into N-bromosuccinimide solution, and then dropwise adding sodium nitrite solution in the presence of cuprous bromide of a catalyst, wherein the temperature is controlled at 1-12 ℃ to obtain the 2, 5-dibromopyridine.
As a further scheme of the invention, after acetone is added in S1, cooling is carried out, the temperature is reduced to-2-3 ℃, then bromine is dropwise added, 20-29ml of acetone is added into 2-aminopyridine per gram, the molar ratio of the 2-aminopyridine to the bromine is 1:1.2-2.6, the reaction temperature is controlled at-8-3 ℃, and the bromine is reacted until the color disappears.
Further, in the S1, N-bromosuccinimide is added in batches in a reaction test, the molar ratio of the N-bromosuccinimide to the 2-aminopyridine is 1:0.6-0.9, the N-bromosuccinimide and the 2-aminopyridine are heated after being added, the reaction temperature is controlled at 2-8 ℃, and the reaction time is 2-6 hours.
Based on the scheme, the acetone is recovered by reduced pressure distillation at the temperature of 3-20 ℃ in the S2, and the pressure is controlled at 20-50Pa, so that a brown yellow solid is obtained.
Further, the mass fraction of the sodium hydroxide solution in the S3 is 16-30%, the stirring and mixing time is 20-40 minutes, and the filtered solid is recrystallized, preferably by using a methanol reagent.
On the basis of the scheme, the temperature of drying in the step S4 is 60-90 ℃.
In still a further embodiment of the present invention, the ratio of 2-amino-5-bromopyridine in S5: n-bromosuccinimide solution: cuprous bromide: the molar ratio of the sodium nitrite solution is 1:2-9: 0.5-3: 0.2-6.
(III) advantageous effects
Compared with the prior art, the invention provides a preparation method of 2, 5-dibromopyridine, which has the following beneficial effects:
1. the preparation method is carried out by taking the 2-aminopyridine as a raw material, the raw material of the 2-aminopyridine is easy to obtain, the cost is low, the reaction condition of the route is mild, the yield is high, the byproducts in the whole process are few, and the method has good industrialization prospect.
2. According to the invention, the reaction efficiency of the N-bromosuccinimide can be improved, the using amount of the N-bromosuccinimide is reduced, the cost is reduced by the steps of adding the N-bromosuccinimide in batches and heating, and the acetone can be recycled by the step of recycling the acetone, so that the cost is reduced.
3. The invention not only reduces the generation of bromide and dibromide through the recrystallization step and the temperature control, but also can improve the yield and the purity of the 2-amino-5-bromopyridine.
Drawings
FIG. 1 is a schematic flow structure diagram of a preparation method of 2, 5-dibromopyridine provided by the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to fig. 1, a method for preparing 2, 5-dibromopyridine comprises the following steps:
s1: mixing and reacting, namely putting 2-aminopyridine into a reactor, adding acetone, and then adding bromization reagents of bromine and N-bromosuccinimide, wherein the raw material of 2-aminopyridine is easy to obtain, the cost is low, the reaction condition of the route is mild, the yield is high, the byproducts in the whole process are few, and the method has good industrialization prospect;
s2: recovering acetone, distilling under reduced pressure to recover acetone, filtering, and collecting the residual solid;
s3: preparing a finished product, namely putting the collected residual solid into a reactor, adding a sodium hydroxide solution, stirring and mixing, and filtering after mixing to obtain 2-amino-5-bromopyridine;
s4: drying, namely drying the obtained 2-amino-5-bromopyridine, and then collecting;
s5: and (2) catalyzing, namely adding 2-amino-5-bromopyridine into an N-bromosuccinimide solution, and then dropwise adding a sodium nitrite solution in the presence of cuprous bromide of a catalyst, wherein the temperature is controlled at 5 ℃ to obtain the 2, 5-dibromopyridine.
According to the invention, acetone is added into S1, then the temperature is reduced to 1 ℃, then bromine is dripped, 22ml of acetone is added into 2-aminopyridine per gram, the molar ratio of 2-aminopyridine to bromine is 1:1.2, the reaction temperature is controlled at-3 ℃, the reaction is carried out until the color of bromine disappears, N-bromosuccinimide is added into the reaction trial in batches in S1, the molar ratio of N-bromosuccinimide to 2-aminopyridine is 1:0.6, heating is carried out after the addition, the reaction temperature is controlled at 3 ℃, the reaction time is 3 hours, and the reaction efficiency of N-bromosuccinimide can be improved, the using amount of N-bromosuccinimide is reduced, and the cost is reduced through the steps of adding N-bromosuccinimide in batches and heating.
Specifically, in S2, acetone is recovered by reduced pressure distillation at 3-20 ℃, the pressure is controlled at 25Pa, a brown yellow solid is obtained, the step of recovering the acetone can be used for recovering and reusing raw materials, the cost is reduced, the mass fraction of a sodium hydroxide solution in S3 is 19%, the stirring and mixing time is 26 minutes, the filtered solid is recrystallized, a methanol reagent is preferably used for recrystallization, the generation of bromide and dibromide is reduced by the recrystallization step and the temperature is controlled, the yield and the purity of 2-amino-5-bromopyridine can be improved, the drying temperature in S4 is 69 ℃, and the drying temperature in S5 is 2-amino-5-bromopyridine: n-bromosuccinimide solution: cuprous bromide: the molar ratio of the sodium nitrite solution is 1:5: 0.9: 3.
example 2
Referring to fig. 1, a method for preparing 2, 5-dibromopyridine comprises the following steps:
s1: mixing and reacting, namely putting 2-aminopyridine into a reactor, adding acetone, and then adding bromization reagents of bromine and N-bromosuccinimide, wherein the raw material of 2-aminopyridine is easy to obtain, the cost is low, the reaction condition of the route is mild, the yield is high, the byproducts in the whole process are few, and the method has good industrialization prospect;
s2: recovering acetone, distilling under reduced pressure to recover acetone, filtering, and collecting the residual solid;
s3: preparing a finished product, namely putting the collected residual solid into a reactor, adding a sodium hydroxide solution, stirring and mixing, and filtering after mixing to obtain 2-amino-5-bromopyridine;
s4: drying, namely drying the obtained 2-amino-5-bromopyridine, and then collecting;
s5: and (2) catalyzing, namely adding 2-amino-5-bromopyridine into an N-bromosuccinimide solution, and then dropwise adding a sodium nitrite solution in the presence of cuprous bromide of a catalyst, wherein the temperature is controlled at 6 ℃ to obtain the 2, 5-dibromopyridine.
According to the invention, acetone is added into S1, then the temperature is reduced to 2 ℃, then bromine is dripped, 23ml of acetone is added into 2-aminopyridine per gram, the molar ratio of 2-aminopyridine to bromine is 1:1.3, the reaction temperature is controlled at-1 ℃, the reaction is carried out until the color of bromine disappears, N-bromosuccinimide is added into the reaction trial in batches in S1, the molar ratio of N-bromosuccinimide to 2-aminopyridine is 1:0.6, heating is carried out after the addition, the reaction temperature is controlled at 3 ℃, the reaction time is 3 hours, and the reaction efficiency of N-bromosuccinimide can be improved, the using amount of N-bromosuccinimide is reduced, and the cost is reduced by adding N-bromosuccinimide in batches and heating.
Specifically, in S2, acetone is recovered by reduced pressure distillation at 3-20 ℃, the pressure is controlled at 30Pa, a brown yellow solid is obtained, the step of recovering the acetone can be used for recovering and reusing raw materials, the cost is reduced, the mass fraction of a sodium hydroxide solution in S3 is 23%, the stirring and mixing time is 29 minutes, the filtered solid is recrystallized, a methanol reagent is preferably used for recrystallization, the generation of bromide and dibromide is reduced by the recrystallization step and the temperature is controlled, the yield and the purity of 2-amino-5-bromopyridine can be improved, the drying temperature in S4 is 69 ℃, and the drying temperature in S5 is 2-amino-5-bromopyridine: n-bromosuccinimide solution: cuprous bromide: the molar ratio of the sodium nitrite solution is 1:5: 0.8: 3.
example 3
Referring to fig. 1, a method for preparing 2, 5-dibromopyridine comprises the following steps:
s1: mixing and reacting, namely putting 2-aminopyridine into a reactor, adding acetone, and then adding bromization reagents of bromine and N-bromosuccinimide, wherein the raw material of 2-aminopyridine is easy to obtain, the cost is low, the reaction condition of the route is mild, the yield is high, the byproducts in the whole process are few, and the method has good industrialization prospect;
s2: recovering acetone, distilling under reduced pressure to recover acetone, filtering, and collecting the residual solid;
s3: preparing a finished product, namely putting the collected residual solid into a reactor, adding a sodium hydroxide solution, stirring and mixing, and filtering after mixing to obtain 2-amino-5-bromopyridine;
s4: drying, namely drying the obtained 2-amino-5-bromopyridine, and then collecting;
s5: and (2) catalyzing, namely adding 2-amino-5-bromopyridine into an N-bromosuccinimide solution, and then dropwise adding a sodium nitrite solution in the presence of cuprous bromide of a catalyst, wherein the temperature is controlled at 5 ℃ to obtain the 2, 5-dibromopyridine.
According to the invention, acetone is added in S1 and then cooled to 1 ℃, then bromine is dripped, 22ml of acetone is added into 2-aminopyridine per gram, the molar ratio of 2-aminopyridine to bromine is 1:1.5, the reaction temperature is controlled to be-8-3 ℃, the reaction is carried out until the color of bromine disappears, N-bromosuccinimide is added in batches in a reaction trial in S1, the molar ratio of N-bromosuccinimide to 2-aminopyridine is 1:0.8, heating is carried out after the addition, the reaction temperature is controlled to be 3 ℃, the reaction time is 3 hours, and the reaction efficiency of N-bromosuccinimide can be improved, the using amount of N-bromosuccinimide is reduced, and the cost is reduced through the steps of adding N-bromosuccinimide in batches and heating.
Specifically, acetone is recovered by reduced pressure distillation at 10 ℃ in S2, the pressure is controlled at 30Pa, a brown yellow solid is obtained, the step of recovering acetone can be used for recovering and reusing raw materials, the cost is reduced, the mass fraction of sodium hydroxide solution in S3 is 23%, the stirring and mixing time is 30 minutes, the filtered solid is recrystallized, methanol reagent is preferably used for recrystallization, the generation of bromide and dibromide is reduced through the step of recrystallization and the temperature is controlled, the yield and the purity of 2-amino-5-bromopyridine can be improved, the drying temperature in S4 is 69 ℃, and the drying temperature in S5 is 2-amino-5-bromopyridine: n-bromosuccinimide solution: cuprous bromide: the molar ratio of the sodium nitrite solution is 1:5: 0.9: 4.
in the description herein, it is noted that relational terms such as first and second, and the like, are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A preparation method of 2, 5-dibromopyridine is characterized by comprising the following steps:
s1: mixing and reacting, namely putting 2-aminopyridine into a reactor, then adding acetone, and then adding a bromization reagent bromine and N-bromosuccinimide;
s2: recovering acetone, distilling under reduced pressure to recover acetone, filtering, and collecting the residual solid;
s3: preparing a finished product, namely putting the collected residual solid into a reactor, adding a sodium hydroxide solution, stirring and mixing, and filtering after mixing to obtain 2-amino-5-bromopyridine;
s4: drying, namely drying the obtained 2-amino-5-bromopyridine, and then collecting;
s5: catalyzing, adding 2-amino-5-bromopyridine into N-bromosuccinimide solution, and then dropwise adding sodium nitrite solution in the presence of cuprous bromide of a catalyst, wherein the temperature is controlled at 1-12 ℃ to obtain the 2, 5-dibromopyridine.
2. The preparation method of 2, 5-dibromopyridine according to claim 1, wherein in S1, acetone is added, then the temperature is reduced to-2-3 ℃, then bromine is added dropwise, 20-29ml of acetone is added to each gram of 2-aminopyridine, the molar ratio of 2-aminopyridine to bromine is 1:1.2-2.6, the reaction temperature is controlled to-8-3 ℃, and the color of bromine is reacted until the color of bromine disappears.
3. The method for preparing 2, 5-dibromopyridine according to claim 2, wherein in S1, N-bromosuccinimide is fed in batches in a reaction test, the molar ratio of N-bromosuccinimide to 2-aminopyridine is 1:0.6-0.9, heating is carried out after feeding, the reaction temperature is controlled at 2-8 ℃, and the reaction time is 2-6 hours.
4. The preparation method of 2, 5-dibromopyridine according to claim 1, wherein acetone is recovered from S2 by distillation under reduced pressure at 3-20 ℃ and the pressure is controlled at 20-50Pa, and a brown yellow solid is obtained.
5. The preparation method of 2, 5-dibromopyridine according to claim 1, wherein the mass fraction of the sodium hydroxide solution in S3 is 16-30%, the stirring and mixing time is 20-40 min, and the filtered solid is recrystallized, preferably by using methanol reagent.
6. The preparation method of 2, 5-dibromopyridine according to claim 5, wherein the temperature for drying in S4 is 60-90 ℃.
7. The method for preparing 2, 5-dibromopyridine according to claim 1, wherein the ratio of 2-amino-5-bromopyridine in S5 is: n-bromosuccinimide solution: cuprous bromide: the molar ratio of the sodium nitrite solution is 1:2-9: 0.5-3: 0.2-6.
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