CN106366009A - Preparation method of chemical intermediate benzocaine - Google Patents
Preparation method of chemical intermediate benzocaine Download PDFInfo
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- CN106366009A CN106366009A CN201610735315.XA CN201610735315A CN106366009A CN 106366009 A CN106366009 A CN 106366009A CN 201610735315 A CN201610735315 A CN 201610735315A CN 106366009 A CN106366009 A CN 106366009A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/12—Formation of amino and carboxyl groups
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/10—Magnesium; Oxides or hydroxides thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/007—Mixed salts
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Abstract
The invention discloses a preparation method of chemical intermediate benzocaine. The preparation method of the chemical intermediate benzocaine comprises the steps: S1, adding 4-nitrobenzoic acid, absolute ethanol, a solid catalyst and a water-carrying agent into a reaction container with a water segregator and performing hot reflux for 1 to 6 hours, wherein the solid catalyst takes magnesium aluminum hydrotalcite as a precursor and modified nanometer bentonite as a carrier, the weight of the precursor is 25 to 45 percent that of the carrier, and the solid catalyst is prepared by grinding and mixing the precursor and the carrier uniformly and calcining at 500 to 700 DEG C for 2 to 4 hours; S2, discharging water out of the water segregator, replenishing the absolute ethanol and continuously performing reflux and water segregation until no water drops occur; S3, after the reaction is finished, filtering when the reaction liquid is hot and putting the filtrate into a hydrogenation kettle to perform hydrogenation reaction; S4, after the hydrogenation is finished, performing heat filtration to remove the catalyst from the system, cooling and filtering under the protection of nitrogen, and drying to obtain the chemical intermediate benzocaine. The preparation method of the benzocaine, provided by the invention, is high in conversion rate; the solid catalyst has high catalytic efficiency and can be repeatedly used, and the catalytic efficiency is not obviously reduced after the catalyst is repeatedly used for 50 times.
Description
Technical field
The invention belongs to chemical field, it is related to chemical intermediate and in particular to a kind of system of chemical intermediate benzocaine
Preparation Method.
Background technology
Benzocaine is a kind of important chemical intermediate, mainly has two kinds of synthetic methods at present: a kind of method is with right
Nitrobenzoic acid is raw material, with concentrated sulphuric acid or cation exchange resin as catalyst with dehydrant, carries out esterification with ethanol
Obtain ethyl p-nitrobenzoate, then obtain benzocaine through iron powder reducing；Another kind of method is then with para-amino benzoic acid
Ethyl ester is raw material, using thionyl chloride, phosphorus oxychloride and concentrated sulphuric acid, is esterified to obtain benzocaine with ethanol.Two methods all exist
, not only to environment, and easily there is etching problem to equipment in the problem that a large amount of spent acid produce, the product obtaining exists
Yield is not high, the problems such as color and luster is bad.
Content of the invention
It is an object of the invention to provide a kind of preparation method of chemical intermediate benzocaine.
The above-mentioned purpose of the present invention is achieved by techniques below scheme:
A kind of preparation method of benzocaine, comprises the steps:
Step s1, in the reaction vessel with water knockout drum add 4- nitrobenzoic acid, dehydrated alcohol, solid catalyst and
Water entrainer, hot reflux 1-6h；With magnesium aluminum-hydrotalcite as precursor, modified Nano bentonite is carrier to described solid catalyst, precursor
Quality is the 25-45% of carrier quality, and precursor and carrier ground and mixed are uniformly obtained final product after 500-700 DEG C of calcining 2-4 hour；
Step s2, releases the moisture in water knockout drum, adds dehydrated alcohol, continues reflux water-dividing and oozes now to anhydrous；
Step s3, after reaction terminates, filtered while hot, filtrate is put into hydrogenation kettle and is carried out hydrogenation reaction；
Step s4, after the completion of hydrogenation, after system heat filters catalyst, cooling under nitrogen protection is filtered, drying；
Wherein, in described magnesium aluminum-hydrotalcite, magnesium elements and the molar ratio of aluminium element are 2-3:1, and preparation method is: by magnesium
Salt and aluminium salt mix and are dissolved in deionized water and be configured to mixing salt solution；Again precipitant is dissolved in deionized water and alkali is obtained
Solution；By gained mixing salt solution and aqueous slkali using and stream mode adds in reaction vessel, then temperature be 40-80 DEG C,
Ph is reaction 30-60 minute under the conditions of 9-11, then stands 8-16 hour, by gained washing of precipitate to neutral, is drying to obtain；
Wherein, described modified Nano bentonite preparation method is: takes nano-bentonite 30-40 part to be scattered in 50-60 part matter
Amount fraction is in the disodium ethylene diamine tetra-acetic acid aqueous solution of 5-15%, stirs 1-2 hour, add 5- under the conditions of 40-50 DEG C
15 parts of zinc sulfate, stir 20-30min, filter, be drying to obtain after cooling.
Preferably, described modified Nano bentonite preparation method is: takes 35 parts of nano-bentonite to be scattered in 55 parts of quality and divides
In the disodium ethylene diamine tetra-acetic acid aqueous solution for 10% for the number, stir 1.5 hours under the conditions of 45 DEG C, add 10 parts of zinc sulfate,
Stirring 25min, filters after cooling, is drying to obtain.
Preferably, in described magnesium aluminum-hydrotalcite preparation method, magnesium salt is magnesium nitrate, magnesium acetate or magnesium sulfate, and aluminium salt is nitric acid
Aluminum, aluminum acetate or aluminum sulfate, precipitant is potassium hydroxide, potassium carbonate, sodium hydroxide or sodium carbonate.
Preferably, described dehydrated alcohol and the mol ratio of 4- nitrobenzoic acid are 0.5-2.5:1.
Preferably, described solid catalyst consumption is the 1-5% of 4- nitrobenzoic acid.
Preferably, described water entrainer is hexamethylene.
Preferably, water entrainer and 4- nitrobenzoic acid mass ratio are 1:4-8.
Preferably, adding dehydrated alcohol amount in step s2 is be initially added dehydrated alcohol amount 0.4-1.0 times.
Advantages of the present invention:
The high conversion rate of benzocaine preparation method of the present invention；Catalysis of solid catalyst efficiency high, can with Reusability, and
After being repeatedly circulated 50 times, catalytic efficiency no substantially reduces.
Specific embodiment
Further illustrate the essentiality content of the present invention with reference to embodiment, but present invention protection model is not limited with this
Enclose.Although being explained in detail to the present invention with reference to preferred embodiment, it will be understood by those within the art that, can be right
Technical scheme is modified or equivalent, without deviating from the spirit and scope of technical solution of the present invention.
In following embodiments, when preparing magnesium aluminum-hydrotalcite, magnesium nitrate selected by magnesium salt, it is possible to use magnesium acetate or magnesium sulfate；
Aluminium salt selects aluminum nitrate, it is possible to use aluminum acetate or aluminum sulfate, and potassium hydroxide selected by precipitant, it is possible to use potassium carbonate, hydrogen-oxygen
Change sodium or sodium carbonate.Prepare water entrainer during benzocaine and use hexamethylene.
Embodiment 1: the preparation of benzocaine
Step s1, in the reaction vessel with water knockout drum add 4- nitrobenzoic acid, dehydrated alcohol, solid catalyst and
Water entrainer, hot reflux 3.5h；With magnesium aluminum-hydrotalcite as precursor, modified Nano bentonite is carrier to described solid catalyst, precursor
Quality is the 35% of carrier quality, and precursor and carrier ground and mixed are uniformly obtained final product after 600 DEG C of calcinings for 3 hours；
Step s2, releases the moisture in water knockout drum, adds dehydrated alcohol, continues reflux water-dividing and oozes now to anhydrous；
Step s3, after reaction terminates, filtered while hot, filtrate is put into hydrogenation kettle and is carried out hydrogenation reaction；
Step s4, after the completion of hydrogenation, after system heat filters catalyst, cooling under nitrogen protection is filtered, drying；
Wherein, in described magnesium aluminum-hydrotalcite, magnesium elements and the molar ratio of aluminium element are 2.5:1, and preparation method is: by magnesium
Salt and aluminium salt mix and are dissolved in deionized water and be configured to mixing salt solution；Again precipitant is dissolved in deionized water and alkali is obtained
Solution；By gained mixing salt solution and aqueous slkali using and stream mode adds in reaction vessel, then temperature be 60 DEG C, ph be
React 45 minutes under the conditions of 10, then stand 12 hours, by gained washing of precipitate to neutral, be drying to obtain；
Wherein, described modified Nano bentonite preparation method is: takes 35 parts of nano-bentonite to be scattered in 55 parts of mass fractions
For, in 10% disodium ethylene diamine tetra-acetic acid aqueous solution, stirring 1.5 hours under the conditions of 45 DEG C, adding 10 parts of zinc sulfate, stir
Mix 25min, filter after cooling, be drying to obtain.
Wherein, described dehydrated alcohol and the mol ratio of 4- nitrobenzoic acid are 1.5:1；Described solid catalyst consumption is 4-
The 3% of nitrobenzoic acid；Described water entrainer and 4- nitrobenzoic acid mass ratio are 1:6；Adding dehydrated alcohol amount in step s2 is
It is initially added 0.7 times of dehydrated alcohol amount.
Embodiment 2: the preparation of benzocaine
Step s1, in the reaction vessel with water knockout drum add 4- nitrobenzoic acid, dehydrated alcohol, solid catalyst and
Water entrainer, hot reflux 1h；With magnesium aluminum-hydrotalcite as precursor, modified Nano bentonite is carrier to described solid catalyst, front body constitution
Measure 25% for carrier quality, precursor and carrier ground and mixed are uniformly obtained final product after 500 DEG C of calcinings for 4 hours；
Step s2, releases the moisture in water knockout drum, adds dehydrated alcohol, continues reflux water-dividing and oozes now to anhydrous；
Step s3, after reaction terminates, filtered while hot, filtrate is put into hydrogenation kettle and is carried out hydrogenation reaction；
Step s4, after the completion of hydrogenation, after system heat filters catalyst, cooling under nitrogen protection is filtered, drying；
Wherein, in described magnesium aluminum-hydrotalcite, magnesium elements and the molar ratio of aluminium element are 2:1, and preparation method is: by magnesium salt
Mix with aluminium salt and be dissolved in deionized water and be configured to mixing salt solution；Again precipitant is dissolved in deionized water and alkali soluble is obtained
Liquid；By gained mixing salt solution and aqueous slkali using and stream mode adds in reaction vessel, then temperature be 40 DEG C, ph be 9
Under the conditions of react 60 minutes, then stand 16 hours, by gained washing of precipitate to neutral, be drying to obtain；
Wherein, described modified Nano bentonite preparation method is: takes 30 parts of nano-bentonite to be scattered in 50 parts of mass fractions
For, in 5% disodium ethylene diamine tetra-acetic acid aqueous solution, stirring 2 hours under the conditions of 40 DEG C, adding 5 parts of zinc sulfate, stirring
20min, filters after cooling, is drying to obtain.
Wherein, described dehydrated alcohol and the mol ratio of 4- nitrobenzoic acid are 0.5:1；Described solid catalyst consumption is 4-
The 1% of nitrobenzoic acid；Described water entrainer and 4- nitrobenzoic acid mass ratio are 1:4；Adding dehydrated alcohol amount in step s2 is
It is initially added 0.4 times of dehydrated alcohol amount.
Embodiment 3: the preparation of benzocaine
Step s1, in the reaction vessel with water knockout drum add 4- nitrobenzoic acid, dehydrated alcohol, solid catalyst and
Water entrainer, hot reflux 6h；With magnesium aluminum-hydrotalcite as precursor, modified Nano bentonite is carrier to described solid catalyst, front body constitution
Measure 45% for carrier quality, precursor and carrier ground and mixed are uniformly obtained final product after 700 DEG C of calcinings for 2 hours；
Step s2, releases the moisture in water knockout drum, adds dehydrated alcohol, continues reflux water-dividing and oozes now to anhydrous；
Step s3, after reaction terminates, filtered while hot, filtrate is put into hydrogenation kettle and is carried out hydrogenation reaction；
Step s4, after the completion of hydrogenation, after system heat filters catalyst, cooling under nitrogen protection is filtered, drying；
Wherein, in described magnesium aluminum-hydrotalcite, magnesium elements and the molar ratio of aluminium element are 3:1, and preparation method is: by magnesium salt
Mix with aluminium salt and be dissolved in deionized water and be configured to mixing salt solution；Again precipitant is dissolved in deionized water and alkali soluble is obtained
Liquid；By gained mixing salt solution and aqueous slkali using and stream mode adds in reaction vessel, then temperature be 80 DEG C, ph be 11
Under the conditions of react 30 minutes, then stand 8 hours, by gained washing of precipitate to neutral, be drying to obtain；
Wherein, described modified Nano bentonite preparation method is: takes 40 parts of nano-bentonite to be scattered in 60 parts of mass fractions
For, in 15% disodium ethylene diamine tetra-acetic acid aqueous solution, stirring 1 hour under the conditions of 50 DEG C, adding 15 parts of zinc sulfate, stirring
30min, filters after cooling, is drying to obtain.
Wherein, described dehydrated alcohol and the mol ratio of 4- nitrobenzoic acid are 2.5:1；Described solid catalyst consumption is 4-
The 5% of nitrobenzoic acid；Described water entrainer and 4- nitrobenzoic acid mass ratio are 1:8；Adding dehydrated alcohol amount in step s2 is
It is initially added 1.0 times of dehydrated alcohol amount.
Embodiment 4: the preparation of benzocaine
Step s1, in the reaction vessel with water knockout drum add 4- nitrobenzoic acid, dehydrated alcohol, solid catalyst and
Water entrainer, hot reflux 3.5h；With magnesium aluminum-hydrotalcite as precursor, modified Nano bentonite is carrier to described solid catalyst, precursor
Quality is the 30% of carrier quality, and precursor and carrier ground and mixed are uniformly obtained final product after 600 DEG C of calcinings for 3 hours；
Step s2, releases the moisture in water knockout drum, adds dehydrated alcohol, continues reflux water-dividing and oozes now to anhydrous；
Step s3, after reaction terminates, filtered while hot, filtrate is put into hydrogenation kettle and is carried out hydrogenation reaction；
Step s4, after the completion of hydrogenation, after system heat filters catalyst, cooling under nitrogen protection is filtered, drying；
Wherein, in described magnesium aluminum-hydrotalcite, magnesium elements and the molar ratio of aluminium element are 2.5:1, and preparation method is: by magnesium
Salt and aluminium salt mix and are dissolved in deionized water and be configured to mixing salt solution；Again precipitant is dissolved in deionized water and alkali is obtained
Solution；By gained mixing salt solution and aqueous slkali using and stream mode adds in reaction vessel, then temperature be 60 DEG C, ph be
React 45 minutes under the conditions of 10, then stand 12 hours, by gained washing of precipitate to neutral, be drying to obtain；
Wherein, described modified Nano bentonite preparation method is: takes 35 parts of nano-bentonite to be scattered in 55 parts of mass fractions
For, in 10% disodium ethylene diamine tetra-acetic acid aqueous solution, stirring 1.5 hours under the conditions of 45 DEG C, adding 10 parts of zinc sulfate, stir
Mix 25min, filter after cooling, be drying to obtain.
Wherein, described dehydrated alcohol and the mol ratio of 4- nitrobenzoic acid are 1.5:1；Described solid catalyst consumption is 4-
The 3% of nitrobenzoic acid；Described water entrainer and 4- nitrobenzoic acid mass ratio are 1:6；Adding dehydrated alcohol amount in step s2 is
It is initially added 0.7 times of dehydrated alcohol amount.
Embodiment 5: the preparation of benzocaine
Step s1, in the reaction vessel with water knockout drum add 4- nitrobenzoic acid, dehydrated alcohol, solid catalyst and
Water entrainer, hot reflux 3.5h；With magnesium aluminum-hydrotalcite as precursor, modified Nano bentonite is carrier to described solid catalyst, precursor
Quality is the 40% of carrier quality, and precursor and carrier ground and mixed are uniformly obtained final product after 600 DEG C of calcinings for 3 hours；
Step s2, releases the moisture in water knockout drum, adds dehydrated alcohol, continues reflux water-dividing and oozes now to anhydrous；
Step s3, after reaction terminates, filtered while hot, filtrate is put into hydrogenation kettle and is carried out hydrogenation reaction；
Step s4, after the completion of hydrogenation, after system heat filters catalyst, cooling under nitrogen protection is filtered, drying；
Wherein, in described magnesium aluminum-hydrotalcite, magnesium elements and the molar ratio of aluminium element are 2.5:1, and preparation method is: by magnesium
Salt and aluminium salt mix and are dissolved in deionized water and be configured to mixing salt solution；Again precipitant is dissolved in deionized water and alkali is obtained
Solution；By gained mixing salt solution and aqueous slkali using and stream mode adds in reaction vessel, then temperature be 60 DEG C, ph be
React 45 minutes under the conditions of 10, then stand 12 hours, by gained washing of precipitate to neutral, be drying to obtain；
Wherein, described modified Nano bentonite preparation method is: takes 35 parts of nano-bentonite to be scattered in 55 parts of mass fractions
For, in 10% disodium ethylene diamine tetra-acetic acid aqueous solution, stirring 1.5 hours under the conditions of 45 DEG C, adding 10 parts of zinc sulfate, stir
Mix 25min, filter after cooling, be drying to obtain.
Wherein, described dehydrated alcohol and the mol ratio of 4- nitrobenzoic acid are 1.5:1；Described solid catalyst consumption is 4-
The 3% of nitrobenzoic acid；Described water entrainer and 4- nitrobenzoic acid mass ratio are 1:6；Adding dehydrated alcohol amount in step s2 is
It is initially added 0.7 times of dehydrated alcohol amount.
Embodiment 6: comparative example, nano-bentonite is not modified
Step s1, in the reaction vessel with water knockout drum add 4- nitrobenzoic acid, dehydrated alcohol, solid catalyst and
Water entrainer, hot reflux 3.5h；With magnesium aluminum-hydrotalcite as precursor, nano-bentonite is carrier to described solid catalyst, precursor mass
For the 35% of carrier quality, precursor and carrier ground and mixed are uniformly obtained final product after 600 DEG C of calcinings for 3 hours；
Step s2, releases the moisture in water knockout drum, adds dehydrated alcohol, continues reflux water-dividing and oozes now to anhydrous；
Step s3, after reaction terminates, filtered while hot, filtrate is put into hydrogenation kettle and is carried out hydrogenation reaction；
Step s4, after the completion of hydrogenation, after system heat filters catalyst, cooling under nitrogen protection is filtered, drying；
Wherein, in described magnesium aluminum-hydrotalcite, magnesium elements and the molar ratio of aluminium element are 2.5:1, and preparation method is: by magnesium
Salt and aluminium salt mix and are dissolved in deionized water and be configured to mixing salt solution；Again precipitant is dissolved in deionized water and alkali is obtained
Solution；By gained mixing salt solution and aqueous slkali using and stream mode adds in reaction vessel, then temperature be 60 DEG C, ph be
React 45 minutes under the conditions of 10, then stand 12 hours, by gained washing of precipitate to neutral, be drying to obtain；
Wherein, described dehydrated alcohol and the mol ratio of 4- nitrobenzoic acid are 1.5:1；Described solid catalyst consumption is 4-
The 3% of nitrobenzoic acid；Described water entrainer and 4- nitrobenzoic acid mass ratio are 1:6；Adding dehydrated alcohol amount in step s2 is
It is initially added 0.7 times of dehydrated alcohol amount.
Embodiment 7: effect example
Urge after the respectively conversion ratio (%) of testing example 1-6 preparation method, and solid catalyst Reusability 40 times
Change the reduction percentage value (%) of efficiency, result is as follows.
| Conversion ratio (%) | Catalytic efficiency reduces percentage rate (%) | |
| Embodiment 1 | 99.6 | 2 |
| Embodiment 6 | 94.3 | 39 |
Embodiment 2-5 measurement result is basically identical with embodiment 1, no longer enumerates one by one.
Result shows, the high conversion rate of benzocaine preparation method of the present invention；Catalysis of solid catalyst efficiency high, can be anti-
Multiple use, and after being repeatedly circulated 50 times, catalytic efficiency no substantially reduces.
The effect of above-described embodiment indicates that the essentiality content of the present invention, but does not limit the protection of the present invention with this
Scope.It will be understood by those within the art that, technical scheme can be modified or equivalent,
Essence without deviating from technical solution of the present invention and protection domain.
Claims (8)
1. a kind of preparation method of benzocaine is it is characterised in that comprise the steps:
Step s1, adds 4- nitrobenzoic acid, dehydrated alcohol, solid catalyst and band water in the reaction vessel with water knockout drum
Agent, hot reflux 1-6h；With magnesium aluminum-hydrotalcite as precursor, modified Nano bentonite is carrier to described solid catalyst, precursor mass
For the 25-45% of carrier quality, precursor and carrier ground and mixed are uniformly obtained final product after 500-700 DEG C of calcining 2-4 hour；
Step s2, releases the moisture in water knockout drum, adds dehydrated alcohol, continues reflux water-dividing and oozes now to anhydrous；
Step s3, after reaction terminates, filtered while hot, filtrate is put into hydrogenation kettle and is carried out hydrogenation reaction；
Step s4, after the completion of hydrogenation, after system heat filters catalyst, cooling under nitrogen protection is filtered, drying；
Wherein, in described magnesium aluminum-hydrotalcite, the molar ratio of magnesium elements and aluminium element is 2-3:1, and preparation method is: by magnesium salt and
Aluminium salt mixes and is dissolved in deionized water and is configured to mixing salt solution；Again precipitant is dissolved in deionized water and alkali soluble is obtained
Liquid；By gained mixing salt solution and aqueous slkali using and stream mode adds in reaction vessel, then temperature be 40-80 DEG C, ph
For reacting 30-60 minute under the conditions of 9-11, then stand 8-16 hour, by gained washing of precipitate to neutral, be drying to obtain；
Wherein, described modified Nano bentonite preparation method is: takes nano-bentonite 30-40 part to be scattered in 50-60 part quality and divides
In the disodium ethylene diamine tetra-acetic acid aqueous solution for 5-15% for the number, stir 1-2 hour under the conditions of 40-50 DEG C, add 5-15 part
Zinc sulfate, stirs 20-30min, filters, be drying to obtain after cooling.
2. preparation method according to claim 1 is it is characterised in that described modified Nano bentonite preparation method is: takes
It is in 10% disodium ethylene diamine tetra-acetic acid aqueous solution that 35 parts of nano-bentonite is scattered in 55 parts of mass fractions, under the conditions of 45 DEG C
Stirring 1.5 hours, adds 10 parts of zinc sulfate, stirs 25min, filters, be drying to obtain after cooling.
3. preparation method according to claim 1 it is characterised in that: in described magnesium aluminum-hydrotalcite preparation method magnesium salt be nitre
Sour magnesium, magnesium acetate or magnesium sulfate, aluminium salt is aluminum nitrate, aluminum acetate or aluminum sulfate, and precipitant is potassium hydroxide, potassium carbonate, hydrogen-oxygen
Change sodium or sodium carbonate.
4. preparation method according to claim 1 it is characterised in that: described dehydrated alcohol and 4- nitrobenzoic acid mole
Than for 0.5-2.5:1.
5. preparation method according to claim 1 it is characterised in that: described solid catalyst consumption be 4- nitrobenzoic acid
1-5%.
6. preparation method according to claim 1 it is characterised in that: described water entrainer be hexamethylene.
7. preparation method according to claim 4 it is characterised in that: water entrainer and 4- nitrobenzoic acid mass ratio are 1:4-
8.
8. preparation method according to claim 1 it is characterised in that: add in step s2 dehydrated alcohol amount be initially added
0.4-1.0 times of dehydrated alcohol amount.
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| CN111732521A (en) * | 2020-06-16 | 2020-10-02 | 浙江优创材料科技股份有限公司 | Preparation method of ethyl p-aminobenzoate |
| CN112526027A (en) * | 2020-12-10 | 2021-03-19 | 南京斯泰尔医药科技有限公司 | RT-HPLC detection method for benzocaine related substances |
| CN118162123A (en) * | 2024-05-11 | 2024-06-11 | 成都理工大学 | Photo-thermal catalytic CO2Hydrogenation catalyst and preparation method thereof |
| CN118162123B (en) * | 2024-05-11 | 2024-07-12 | 成都理工大学 | Photo-thermal catalytic CO2Hydrogenation catalyst and preparation method thereof |
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