CN112679366A - Purification method of N- (2-aminoethyl) -N-ethyl m-toluidine - Google Patents
Purification method of N- (2-aminoethyl) -N-ethyl m-toluidine Download PDFInfo
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- CN112679366A CN112679366A CN202011472022.XA CN202011472022A CN112679366A CN 112679366 A CN112679366 A CN 112679366A CN 202011472022 A CN202011472022 A CN 202011472022A CN 112679366 A CN112679366 A CN 112679366A
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Abstract
The application relates to the technical field of purification of unsymmetrical substituted ethylene diamine, and particularly discloses a purification method of N- (2-aminoethyl) -N-ethyl m-toluidine, which comprises the following steps: adding ethyl acetate into the crude product of the N- (2-aminoethyl) -N-ethyl m-toluidine, uniformly mixing, and heating to obtain an oil-water mixture; standing and cooling the oil-water mixture to separate out crystals in the oil-water mixture, and then performing pressure filtration for 1-2 hours under the control of the vacuum degree of-0.09 to-0.06 Mpa to obtain a primary filter cake and a primary filter liquor; adding ethanol into the obtained primary filter cake, uniformly mixing, and then heating to obtain a first mixture; adding ethyl acetate into the first mixture, uniformly mixing, and stirring to obtain a second mixture; and carrying out secondary filter pressing on the obtained mixture, standing and cooling the obtained filtrate, controlling filter pressing, and drying the filter cake obtained by filter pressing to obtain the refined product of the N- (2-aminoethyl) -N-ethyl m-toluidine. The purification method has the advantages of simple operation and higher yield and purity of the final product.
Description
Technical Field
The application relates to the technical field of purification of unsymmetrically substituted ethylene diamine, in particular to a method for purifying N- (2-aminoethyl) -N-ethyl m-toluidine.
Background
The molecular terminal of the N- (2-aminoethyl) -N-ethyl m-toluidine has amino group, contains lone pair electrons, is a good nucleophilic reagent, can react with halohydrocarbon, carboxylic acid, anhydride, acyl chloride and the like, and has important application in the fields of dye and medicine.
Under the conditions of normal temperature and normal pressure, the boiling point of N- (2-aminoethyl) -N-ethyl m-toluidine is near 300 ℃, the boiling point is high, in the related technology, the method is generally used for separating and purifying the N- (2-aminoethyl) -N-ethyl m-toluidine by adopting a reduced pressure distillation mode, but the method has high requirement on vacuum degree, further has high requirement on pressure resistance of equipment, and meanwhile, the yield of the product is low and is about 50 percent. Meanwhile, in order to ensure the purity of the product, the vacuum degree also needs to be kept stable in the separation process. And therefore the operating requirements are high.
In view of the above-mentioned related art, the inventors thought that there were disadvantages that the requirements for the equipment required for purification were high and the conditions required for purification were severe.
Disclosure of Invention
In order to improve the purification yield and purity of the N- (2-aminoethyl) -N-ethyl m-toluidine product and ensure the simplicity of purification operation conditions, the application provides a purification method of N- (2-aminoethyl) -N-ethyl m-toluidine.
The purification method of N- (2-aminoethyl) -N-ethyl m-toluidine provided by the application adopts the following technical scheme:
a process for the purification of N- (2-aminoethyl) -N-ethyl-m-toluidine comprising the steps of:
(1) adding ethyl acetate into the crude product of the N- (2-aminoethyl) -N-ethyl m-toluidine, uniformly mixing, and keeping the temperature at 70-80 ℃ for 15-30 min to obtain an oil-water mixture;
(2) standing the oil-water mixture obtained in the step (1) for 10-15 hours at the temperature of 5-15 ℃ to separate out crystals from the oil-water mixture, and then performing pressure filtration for 1-2 hours under the vacuum degree of-0.09 to-0.06 MPa to obtain a primary filter cake and a primary filter liquor;
(3) adding ethanol into the primary filter cake obtained in the step (2), uniformly mixing, and then keeping the temperature at 70-80 ℃ for 15-30 min to obtain a first mixture;
(4) adding ethyl acetate into the mixture I in the step (3), uniformly mixing, and stirring for 5-10 min at the rotation speed of 250-350 r/min to obtain a mixture II;
(5) and (3) performing filter pressing on the mixture II obtained in the step (4) for 3min to 5min under the condition that the vacuum degree is controlled to be-0.09 to-0.06 Mpa, standing the obtained filtrate for 10h to 15h under the condition that the temperature is controlled to be 5 ℃ to 15 ℃, then performing filter pressing for 5min to 10min under the condition that the vacuum degree is controlled to be-0.09 to-0.06 Mpa, and drying the filter cake obtained by filter pressing for 5h to 8h under the condition that the temperature is controlled to be 50 ℃ to 60 ℃ to obtain the refined product of the N- (2-aminoethyl) -N-ethyl m-toluidine.
By adopting the technical scheme, the ethyl acetate is poor solvent for the N- (2-aminoethyl) -N-ethyl m-toluidine, so that the addition of the ethyl acetate in the step (1) can promote the precipitation of the N- (2-aminoethyl) -N-ethyl m-toluidine, namely promote the recrystallization of the N- (2-aminoethyl) -N-ethyl m-toluidine and dissolve impurities in the crude product of the N- (2-aminoethyl) -N-ethyl m-toluidine into the ethyl acetate, thereby removing most impurities in the crude product of the N- (2-aminoethyl) -N-ethyl m-toluidine by pressure filtration; and the ethanol is a good solvent for the N- (2-aminoethyl) -N-ethyl m-toluidine, the addition of the ethanol only is not beneficial to separating solid N- (2-aminoethyl) -N-ethyl m-toluidine from the mixture II in the step (5), the addition of the ethyl acetate can promote the mixture II to separate the N- (2-aminoethyl) -N-ethyl m-toluidine, and then impurities dissolved in the ethanol and the ethyl acetate in the mixture II are removed through pressure filtration, so that the N- (2-aminoethyl) -N-ethyl m-toluidine with higher purity can be obtained, and the operation can also improve the yield of the refined product of the N- (2-aminoethyl) -N-ethyl m-toluidine.
Preferably, the ratio of the crude N- (2-aminoethyl) -N-ethyl-m-toluidine in the step (1) to the ethyl acetate in the step (1) is 1-1.8 g:1ml by mass: volume.
By adopting the technical scheme, the purity of the finally obtained N- (2-aminoethyl) -N-ethyl m-toluidine refined product can reach 99.15% -99.48%.
Preferably, the ratio of the dosage of the primary filter cake to the ethanol is 1.5-2.5 g to 1ml by mass to volume.
By adopting the technical scheme, the filter cake can be fully dissolved after being filtered once, and in the proportion range of the using amount, the problem that the crystallization is not easy to occur in the solution due to excessive ethanol can be solved, so that the final yield of the purification method of the N- (2-aminoethyl) -N-ethyl m-toluidine in the application reaches 70.7% -73.5%.
Preferably, the ratio of the dosage of the primary filter cake to the ethanol is 1.5-2.04 g to 1ml by mass to volume.
By adopting the technical scheme, the final yield of the purification method of the N- (2-aminoethyl) -N-ethyl m-toluidine in the application can reach 71.8% -73.5%.
Preferably, the ratio of the dosage of the once-filtration filter cake to the ethanol is 1.5g to 1ml by mass to volume.
By adopting the technical scheme, the final yield of the purification method of the N- (2-aminoethyl) -N-ethyl m-toluidine in the application can reach 73.5%.
Preferably, the volume ratio of the ethanol to the ethyl acetate in the step (4) is 0.8-1.2: 1.
By adopting the technical scheme, the purity of the finally obtained N- (2-aminoethyl) -N-ethyl m-toluidine refined product can reach 99.15% -99.48%.
Preferably, the ratio of the ethanol to the ethyl acetate in the step (4) is 0.8-1: 1 by volume.
By adopting the technical scheme, the purity of the finally obtained N- (2-aminoethyl) -N-ethyl m-toluidine refined product can be improved to 99.22% -99.48%.
Preferably, the ratio of the ethanol to the ethyl acetate in the step (4) is 0.8:1 in terms of volume ratio.
By adopting the technical scheme, the purity of the finally obtained N- (2-aminoethyl) -N-ethyl m-toluidine refined product can be improved to 99.48 percent.
In summary, the present application has the following beneficial effects:
1. because the method adopts twice recrystallization and vacuum filtration, the difficulty of purification operation is reduced, the yield can be obviously improved, and the requirement on reaction equipment is lower because the vacuum degree of filter pressing is only-0.09 to-0.06 MPa and the heating temperature is only 50 to 80 ℃;
2. in the method, ethanol and ethyl acetate are used as a mixed solvent for secondary recrystallization, so that compared with the method of simply using ethyl acetate, the purity of the finally obtained N- (2-aminoethyl) -N-ethyl m-toluidine refined product can reach 99.15-99.48%, and the yield reaches 70.7-73.5%; in particular, when the ratio of ethanol to ethyl acetate is 0.8:1, the purity of the finally obtained purified N- (2-aminoethyl) -N-ethyl-m-toluidine product can be 99.48%.
Drawings
Fig. 1 is a flow chart of a method provided herein.
Detailed Description
The present application will be described in further detail with reference to the following examples and accompanying drawings.
In each example, the purity was determined by the following method: the product was tested by liquid chromatography (HPLC) and the HPLC purity of the product N- (2-aminoethyl) -N-ethyl-m-toluidine was determined by peak area normalization.
The yield of the purified N- (2-aminoethyl) -N-ethyl-m-toluidine product prepared in each example was calculated as follows: yield = mass of product/(molar mass charged of N-ethyl-m-toluidine × molar mass of N- (2-aminoethyl) -N-ethyl-m-toluidine) × 100%.
The raw material specifications and the manufacturer information used in the examples and comparative examples of the present application are commercially available unless otherwise specified:
n-ethyl m-toluidine, manufacturer: shanghai Aladdin Biotechnology Ltd.
The equipment model and the manufacturer information used in the embodiments of the present application are as follows:
magnetic stirrers, model: DF-101S heat collection type constant temperature heating magnetic stirrer; the manufacturer: consolidate City Prohua instruments, Inc.;
high performance liquid chromatograph: the model is as follows: alliance e 2695; the manufacturer: waters Corporation.
Preparation of a crude product of aminoethyl) -N-ethyl-m-toluidine
Preparation example 1
The preparation method comprises the following steps: 0.1mol (13.52 g) of N-ethyl-m-toluidine, 0.11mol (22.54 g) of 2-bromoethylamine hydrobromide, 0.07mol (7 g) of calcium carbonate and 7.5mL of water were sequentially charged into a 250mL three-necked flask equipped with a thermometer, a condenser and a magnetic stirrer, and then the contents of the flask were stirred at 300r/min and heated to 140 ℃ for reflux reaction for 4 hours, followed by natural cooling to room temperature to obtain 50.2g of a crude product of N- (2-aminoethyl) -N-ethyl-m-toluidine having a purity of 92.70%.
Preparation example 2
The preparation method comprises the following steps: 0.1mol (13.52 g) of N-ethyl-m-toluidine, 0.11mol (22.54 g) of 2-bromoethylamine hydrobromide, 0.07mol (7 g) of calcium carbonate and 7.5mL of water were sequentially charged into a 250mL three-necked flask equipped with a thermometer, a condenser and a magnetic stirrer, and then the contents of the flask were stirred at 300r/min and heated to 140 ℃ for reflux reaction for 4 hours, followed by natural cooling to room temperature to obtain 50g of a crude product having a purity of 90% of N- (2-aminoethyl) -N-ethyl-m-toluidine.
Preparation example 3
The preparation method comprises the following steps: 0.1mol (13.52 g) of N-ethyl-m-toluidine, 0.11mol (22.54 g) of 2-bromoethylamine hydrobromide, 0.07mol (7 g) of calcium carbonate and 7.5mL of water were sequentially charged into a 250mL three-necked flask equipped with a thermometer, a condenser and a magnetic stirrer, and then the contents of the flask were stirred at 300r/min and heated to 140 ℃ for reflux reaction for 4 hours, followed by natural cooling to room temperature to obtain 49.5g of a crude product of N- (2-aminoethyl) -N-ethyl-m-toluidine having a purity of 93%.
Examples
Example 1
A process for the purification of N- (2-aminoethyl) -N-ethyl-m-toluidine comprising the steps of:
(1) adding 40ml of ethyl acetate into a crude product of N- (2-aminoethyl) -N-ethyl m-toluidine with the purity of 92.70 percent and the mass of 50.2g, uniformly mixing, and keeping the temperature at 75 ℃ for 20min to obtain an oil-water mixture;
(2) standing the oil-water mixture in the step (1) for 10 hours at the temperature of 10 ℃ to separate out solids from the oil-water mixture, and then performing pressure filtration for 1 hour under the vacuum degree of-0.07 Mpa to obtain a primary filtration cake and a primary filtration filtrate, wherein the mass of the primary filtration cake is 25.5 g;
(3) adding 12.5ml of ethanol into the primary filter cake obtained in the step (2), uniformly mixing, and then keeping the temperature at 75 ℃ for 20min to obtain a first mixture;
(4) adding 12.5ml of ethyl acetate into the mixture I in the step (3), uniformly mixing, and stirring for 7min at the rotation speed of 300r/min to obtain a mixture II;
(5) and (3) performing pressure filtration on the mixture II obtained in the step (4) for 3min under the condition that the vacuum degree is controlled to be-0.07 Mpa, standing the obtained filtrate for 10h under the condition that the temperature is controlled to be 10 ℃, performing pressure filtration for 5min under the condition that the vacuum degree is controlled to be-0.07 Mpa, and drying the filter cake obtained by pressure filtration for 5h under the condition that the temperature is controlled to be 55 ℃ to obtain 12.6g of refined N- (2-aminoethyl) -N-ethyl m-toluidine with the purity of 99.22 percent, wherein the yield is 70.7 percent.
In the step (1) of the above example, the amount ratio of the crude N- (2-aminoethyl) -N-ethyl-m-toluidine to ethyl acetate was 1.255g:1 ml.
In the step (3) of the above example, the ratio of the amount of the filter cake to ethanol was once filtered, and the ratio of the filter cake to ethanol was 2.04 g:1 ml.
The ratio of the ethanol in step (3) to the ethyl acetate in step (4) in the above examples is 1:1 by volume.
Example 2
A process for the purification of N- (2-aminoethyl) -N-ethyl-m-toluidine comprising the steps of:
(1) adding 50.0ml ethyl acetate into crude product of N- (2-aminoethyl) -N-ethyl m-toluidine with purity of 90% and mass of 50.0g, mixing uniformly, and keeping at 70 deg.C for 15min to obtain oil-water mixture;
(2) standing the oil-water mixture in the step (1) for 13 hours at the temperature of 5 ℃ to separate out solids from the oil-water mixture, and then performing pressure filtration for 1.5 hours under the vacuum degree of-0.06 Mpa to obtain a primary filtration cake and a primary filtration filtrate, wherein the mass of the primary filtration cake is 24.6 g;
(3) adding 16.4ml of ethanol into the primary filter cake obtained in the step (2), uniformly mixing, and then keeping the temperature at 70 ℃ for 15min to obtain a first mixture;
(4) adding 20.5ml of ethyl acetate into the mixture I in the step (3), uniformly mixing, and stirring for 5min at the rotation speed of 250r/min to obtain a mixture II;
(5) and (3) performing pressure filtration on the mixture II obtained in the step (4) for 4min under the condition that the vacuum degree is controlled to be-0.06 Mpa, standing the obtained filtrate for 13h under the condition that the temperature is controlled to be 5 ℃, performing pressure filtration for 8min under the condition that the vacuum degree is controlled to be-0.06 Mpa, and drying a filter cake obtained by pressure filtration for 6.5h under the condition that the temperature is controlled to be 50 ℃ to obtain 13.1g of N- (2-aminoethyl) -N-ethyl m-toluidine refined product with the purity of 99.48 percent, wherein the yield is 73.5 percent.
In the step (1) of the above example, the amount ratio of the crude N- (2-aminoethyl) -N-ethyl-m-toluidine to ethyl acetate was 1 g:1 ml.
In the step (3) of the above example, the ratio of the amount of the filter cake to ethanol used in one filtration was 1.5 g:1 ml.
The ratio of the ethanol in step (3) to the ethyl acetate in step (4) in the above examples is 0.8:1 by volume.
Example 3
A process for the purification of N- (2-aminoethyl) -N-ethyl-m-toluidine comprising the steps of:
(1) adding 27.5ml of ethyl acetate into a crude product of N- (2-aminoethyl) -N-ethyl m-toluidine with the purity of 93 percent and the mass of 49.5g, uniformly mixing, and keeping the temperature at 80 ℃ for 30min to obtain an oil-water mixture;
(2) standing the oil-water mixture in the step (1) for 15h at the temperature of 15 ℃ to separate out solids from the oil-water mixture, and then performing pressure filtration for 2h under the vacuum degree of-0.09 Mpa to obtain a primary filtration cake and a primary filtration filtrate, wherein the mass of the primary filtration cake is 27.0 g;
(3) adding 10.8ml of ethanol into the primary filter cake obtained in the step (2), uniformly mixing, and then keeping the temperature at 80 ℃ for 30min to obtain a first mixture;
(4) adding 9.0ml of ethyl acetate into the mixture I in the step (3), uniformly mixing, and stirring for 10min at the rotation speed of 350r/min to obtain a mixture II;
(5) and (3) performing pressure filtration on the mixture II obtained in the step (4) for 5min under the condition that the vacuum degree is controlled to be-0.09 Mpa, standing the obtained filtrate for 15h under the condition that the temperature is controlled to be 15 ℃, performing pressure filtration for 10min under the condition that the vacuum degree is controlled to be-0.09 Mpa, and drying a filter cake obtained by pressure filtration for 8h under the condition that the temperature is controlled to be 60 ℃ to obtain 12.8g of N- (2-aminoethyl) -N-ethyl m-toluidine refined product with the purity of 99.15 percent, wherein the yield is 71.8 percent.
In the step (1) of the above example, the amount ratio of the crude N- (2-aminoethyl) -N-ethyl-m-toluidine to ethyl acetate was 1.8 g:1 ml.
In the step (3) of the above example, the ratio of the amount of the filter cake to ethanol was once filtered, and the ratio of the filter cake to ethanol was 2.5g to 1 ml.
The ratio of the ethanol in step (3) to the ethyl acetate in step (4) in the above examples is 1.2:1 by volume.
Comparative example
Comparative example 1
A process for the purification of N- (2-aminoethyl) -N-ethyl-m-toluidine comprising the steps of:
(1) adding 50.0ml ethyl acetate into crude product of N- (2-aminoethyl) -N-ethyl m-toluidine with purity of 90% and mass of 50.0g, mixing uniformly, and keeping at 70 deg.C for 15min to obtain oil-water mixture;
(2) standing the oil-water mixture in the step (1) for 13 hours at the temperature of 5 ℃ to separate out solids from the oil-water mixture, and then performing pressure filtration for 1.5 hours under the vacuum degree of-0.06 Mpa to obtain a primary filtration cake and a primary filtration filtrate, wherein the mass of the primary filtration cake is 24.6 g;
(3) adding 20.5ml of ethyl acetate into the primary filter cake obtained in the step (2), uniformly mixing, keeping the temperature at 70 ℃ for 15min, and stirring at the rotation speed of 250r/min for 5min to obtain a first mixture;
(4) and (3) controlling the vacuum degree of the mixture I obtained in the step (3) to be-0.06 Mpa, carrying out filter pressing for 4min, controlling the temperature of the obtained filtrate to be 5 ℃, standing for 13h, then controlling the vacuum degree to be-0.06 Mpa, carrying out filter pressing for 8min, controlling the temperature of the filter cake obtained by filter pressing to be 50 ℃, and drying for 6.5h to obtain 14.2g of N- (2-aminoethyl) -N-ethyl m-toluidine refined product with the purity of 95.24%, wherein the yield is 79.6%.
In the step (1) of the above example, the amount ratio of the crude N- (2-aminoethyl) -N-ethyl-m-toluidine to ethyl acetate was 1 g:1 ml.
Comparative example 2
A process for the purification of N- (2-aminoethyl) -N-ethyl-m-toluidine comprising the steps of:
(1) adding 50.0ml ethyl acetate into crude product of N- (2-aminoethyl) -N-ethyl m-toluidine with purity of 90% and mass of 50.0g, mixing uniformly, and keeping at 70 deg.C for 15min to obtain oil-water mixture;
(2) standing the oil-water mixture in the step (1) for 13 hours at the temperature of 5 ℃ to separate out solids from the oil-water mixture, and then performing pressure filtration for 1.5 hours under the vacuum degree of-0.06 Mpa to obtain a primary filtration cake and a primary filtration filtrate, wherein the mass of the primary filtration cake is 24.6 g;
(3) adding 36.9ml of ethyl acetate into the primary filter cake obtained in the step (2), uniformly mixing, keeping the temperature at 70 ℃ for 15min, and stirring at the rotation speed of 250r/min for 5min to obtain a first mixture;
(4) and (3) controlling the vacuum degree of the mixture I obtained in the step (3) to be-0.06 Mpa, carrying out filter pressing for 4min, controlling the temperature of the obtained filtrate to be 5 ℃, standing for 13h, then controlling the vacuum degree to be-0.06 Mpa, carrying out filter pressing for 8min, controlling the temperature of a filter cake obtained by filter pressing to be 50 ℃, and drying for 6.5h to obtain 13.9g of refined N- (2-aminoethyl) -N-ethyl m-toluidine product with the purity of 97.64 percent, wherein the yield is 78.0 percent.
In the step (1) of the above example, the amount ratio of the crude N- (2-aminoethyl) -N-ethyl-m-toluidine to ethyl acetate was 1 g:1 ml.
As can be seen by combining comparative example 1 with comparative example 2 and combining example 2, the purity of example 2 in which ethanol and ethyl acetate were added together to the primary filtration cake was higher than that of comparative example 1 and comparative example 2 in which only ethyl acetate was added, and it can be seen that the purity of the refined product of N- (2-aminoethyl) -N-ethyl-m-toluidine was improved by adding ethanol and ethyl acetate together to the primary filtration cake.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (8)
1. A method for purifying N- (2-aminoethyl) -N-ethyl-m-toluidine, which comprises the following steps:
(1) adding ethyl acetate into the crude product of the N- (2-aminoethyl) -N-ethyl m-toluidine, uniformly mixing, and keeping the temperature at 70-80 ℃ for 15-30 min to obtain an oil-water mixture;
(2) standing the oil-water mixture obtained in the step (1) for 10-15 hours at the temperature of 5-15 ℃ to separate out crystals from the oil-water mixture, and then performing pressure filtration for 1-2 hours under the vacuum degree of-0.09 to-0.06 MPa to obtain a primary filter cake and a primary filter liquor;
(3) adding ethanol into the primary filter cake obtained in the step (2), uniformly mixing, and then keeping the temperature at 70-80 ℃ for 15-30 min to obtain a first mixture;
(4) adding ethyl acetate into the mixture I in the step (3), uniformly mixing, and stirring for 5-10 min at the rotation speed of 250-350 r/min to obtain a mixture II;
(5) and (3) performing filter pressing on the mixture II obtained in the step (4) for 3min to 5min under the condition that the vacuum degree is controlled to be-0.09 to-0.06 Mpa, standing the obtained filtrate for 10h to 15h under the condition that the temperature is controlled to be 5 ℃ to 15 ℃, then performing filter pressing for 5min to 10min under the condition that the vacuum degree is controlled to be-0.09 to-0.06 Mpa, and drying the filter cake obtained by filter pressing for 5h to 8h under the condition that the temperature is controlled to be 50 ℃ to 60 ℃ to obtain the refined product of the N- (2-aminoethyl) -N-ethyl m-toluidine.
2. The method for purifying N- (2-aminoethyl) -N-ethyl-m-toluidine according to claim 1, wherein: the ratio of the N- (2-aminoethyl) -N-ethyl-m-toluidine crude product in the step (1) to the ethyl acetate in the step (1) is 1-1.8 g:1ml by mass: volume.
3. The method for purifying N- (2-aminoethyl) -N-ethyl-m-toluidine according to claim 1, wherein: the ratio of the dosage of the primary filter cake to the ethanol is calculated according to the mass to the volume, and the ratio of the primary filter cake to the ethanol is 1.5-2.5 g to 1 ml.
4. The method according to claim 3, wherein the purification of N- (2-aminoethyl) -N-ethyl-m-toluidine comprises: the ratio of the dosage of the primary filter cake to the ethanol is calculated according to the mass to the volume, and the ratio of the primary filter cake to the ethanol is 1.5-2.04 g to 1 ml.
5. The method according to claim 4, wherein the purification of N- (2-aminoethyl) -N-ethyl-m-toluidine comprises: the ratio of the dosage of the primary filter cake to the ethanol is calculated according to the mass to the volume, and the ratio of the primary filter cake to the ethanol is 1.5g to 1 ml.
6. The method for purifying N- (2-aminoethyl) -N-ethyl-m-toluidine according to claim 1, wherein: the volume ratio of the ethanol to the ethyl acetate in the step (4) is 0.8-1.2: 1.
7. The method according to claim 6, wherein the purification of N- (2-aminoethyl) -N-ethyl-m-toluidine comprises: the ratio of the ethanol to the ethyl acetate in the step (4) is 0.8-1: 1 by volume.
8. The method according to claim 7, wherein the purification of N- (2-aminoethyl) -N-ethyl-m-toluidine comprises: the ratio of the ethanol to the ethyl acetate in the step (4) is 0.8:1 by volume.
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Application publication date: 20210420 |