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Purification method of N-(2-aminoethyl)-N-ethyl m-toluidine

A purification method and technology of toluidine, applied in amino compound purification/separation, organic chemistry, etc., can solve the problems of high equipment requirements for purification, harsh conditions for purification, etc., and achieve the effect of reducing difficulty and increasing yield

Inactive Publication Date: 2021-04-20
上海俪源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In view of the above-mentioned related technologies, the inventor believes that there is a defect that the requirements for the equipment required for purification are relatively high, and the conditions required for purification are relatively harsh.

Method used

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  • Purification method of N-(2-aminoethyl)-N-ethyl m-toluidine

Examples

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Effect test

preparation example 1

[0042] Preparation method: Add 0.1mol (13.52g) N-ethyl-m-toluidine, 0.11mol (22.54g) 2-bromoethylamine hydrobromide to a 250mL three-necked flask equipped with a thermometer, condenser and magnetic stirrer Salt, 0.07mol (7g) calcium carbonate and 7.5ml water, then stir the material in the flask at a speed of 300r / min, and raise the temperature to 140°C, reflux for 4h, and then naturally cool to room temperature to obtain a purity of 92.70%N - 50.2 g of crude product of (2-aminoethyl)-N-ethyl-m-toluidine.

preparation example 2

[0044]Preparation method: Add 0.1mol (13.52g) N-ethyl-m-toluidine, 0.11mol (22.54g) 2-bromoethylamine hydrobromide to a 250mL three-necked flask equipped with a thermometer, condenser and magnetic stirrer Salt, 0.07mol (7g) calcium carbonate and 7.5ml water, then stir the material in the flask at a speed of 300r / min, and raise the temperature to 140°C, reflux for 4h, and then naturally cool to room temperature to obtain a purity of 90% N - 50 g of a crude product of (2-aminoethyl)-N-ethyl-m-toluidine.

preparation example 3

[0046] Preparation method: Add 0.1mol (13.52g) N-ethyl-m-toluidine, 0.11mol (22.54g) 2-bromoethylamine hydrobromide to a 250mL three-necked flask equipped with a thermometer, condenser and magnetic stirrer Salt, 0.07mol (7g) calcium carbonate and 7.5ml water, then stir the material in the flask at a speed of 300r / min, and raise the temperature to 140°C, reflux for 4h, and then naturally cool to room temperature to obtain a purity of 93% N - 49.5 g of crude product of (2-aminoethyl)-N-ethyl-m-toluidine.

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Abstract

The invention relates to the technical field of purification of asymmetric substituted ethylenediamine, and particularly discloses a purification method of N-(2-aminoethyl)-N-ethyl m-toluidine, which comprises the following steps: adding ethyl acetate into an N (2-aminoethyl)-N-ethyl m-toluidine crude product, uniformly mixing, and heating to obtain an oil-water mixture; performing standing and cooling the oil-water mixture to separate out crystals from the oil-water mixture, and then controlling the vacuum degree to be -0.09-0.06 Mpa for filter pressing for 1 hour to 2 hours to obtain a primary filter cake and primary filter liquor; adding ethanol into the obtained primary filter cake, uniformly mixing, and then heating to obtain a mixture I; adding ethyl acetate into the mixture I, uniformly mixing, and stirring to obtain a mixture II; and carrying out pressure filtration on the obtained mixture II, standing and cooling the obtained filtrate, carrying out pressure filtration under control, and drying the filter cake obtained by pressure filtration to obtain the N (2-aminoethyl)-N-ethyl-m-toluidine refined product. The purification method provided by the invention has the advantages of simple operation and high yield and purity of the final product.

Description

technical field [0001] The application relates to the technical field of purification of asymmetrically substituted ethylenediamine, more specifically, it relates to a purification method of N-(2-aminoethyl)-N-ethyl m-toluidine. Background technique [0002] N-(2-aminoethyl)-N-ethyl m-toluidine has an amino group at the end of the molecule and contains a lone pair of electrons. It is a good nucleophile and can be used with halogenated hydrocarbons, carboxylic acids, acid anhydrides, Acyl chloride reacts, and has important applications in the fields of dyes and medicine. [0003] Under normal temperature and normal pressure conditions, the boiling point of N-(2-aminoethyl)-N-ethyl-m-toluidine is nearly 300°C, which is high. In related technologies, vacuum distillation is generally used to separate and purify it , but this method has high requirements for vacuum degree, and further requires high pressure resistance capability of equipment, and the yield of product is low at a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/84C07C211/53
Inventor 刘子轩章燕琴
Owner 上海俪源科技有限公司
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