A method of obtaining a (n, n'- tetramethylethylenediamine) copper sulfate pentahydrate

 

(57) Abstract:

The invention relates to the field of organic chemistry, in particular to a method for (N,N'-tetramethylethylenediamine) copper sulfate pentahydrate, which can be used as a growth promoter and plant productivity. The method consists in the interaction of an aqueous solution of dimethylamine with formalin and then adding an aqueous solution of oxalic acid and copper sulfate pentahydrate at a temperature of 21-22oC for 2-4 hours-Difference method is that the molar ratio of the starting components is(2-2,1):(1-1,1):1:1. The technical result is simplification. table 1.

The invention relates to organic chemistry, specifically to an improved method for producing a (N,N'-tetramethylethylenediamine) copper sulfate pentahydrate General formula

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(N, N'-tetramethylethylenediamine) copper sulfate pentahydrate can be used as a growth promoter and plant productivity.

There is a method /auth.St. 1786020 the USSR (1992), BI N 1 (1993)/ N, N'-tetramethylmethylenediamine acetic acid reaction tetramethylmethylenediamine (2) with equimolar to obtain (N,N'-tetramethylethylenediamine) copper sulfate pentahydrate formula (1).

A method of obtaining /auth.St. 1766349 the USSR (1990), BI (N) 37 (1992)/ (N, N'-tetramethylethylenediamine) copper sulfate pentahydrate (1) reaction of tetramethylethylenediamine (2) with equimolar amount of an aqueous solution of oxalic acid at a temperature of 20-25oC for 1 hour followed by the addition of copper sulfate pentahydrate (3) and stirring the reaction mixture for 2 hours. Source tetramethylmethylenediamine (2) previously obtained by reaction of the amine with formaldehyde, followed by extraction with isopentane and separation from the solvent using a rectification column. These reactions proceed according to the scheme

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The disadvantage of this method is to obtain the target product (1) in three stages:

a) obtaining a source tetramethylmethylenediamine (2) by the interaction of the amine with formaldehyde and subsequent extraction (2) using boiling solvents and separation (2) from the solvent rectification column;

b) obtaining N, N'-tetramethylmethylenediamine (4) the interaction of tetramethylethylenediamine (2) with an aqueous solution of oxalic acid;

C) obtaining (N,N'-tetramethylmethylenediamine the pentahydrate of copper sulfate (3).

Offers an improved way to obtain (N,N'-tetramethylethylenediamine) copper sulfate pentahydrate formula (1).

The method consists in the interaction of an aqueous solution of dimethylamine (CH3)2NH with formalin (CH2O) followed by the addition at a temperature of 21-22oC aqueous solution of oxalic acid (COOH)2and copper sulfate pentahydrate CuSO45H2O, taken in a molar ratio (CH3)2NH:(CH2O):(COOH)2: CuSO45H2O= (2-2,1):(1-1,1):1:1 and stirring the reaction mixture for 2-4 hours. Output (N,N'-tetramethylethylenediamine) copper sulfate pentahydrate is 95-100%.

The reaction proceeds in one stage scheme

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Source dimethylamine and formaldehyde take in a small excess with respect to oxalic acid and CuSO45H2O that is associated with the volatility of dimethylamine and formaldehyde from their aqueous solutions. The reaction is preferably carried out at a temperature of 21-22oC, because at higher temperatures, for example 50oC, increases the volatility of dimethylamine and formaldehyde from their aqueous solutions; at lower temperatures, for example 0oC, decreases the reaction rate.

3)2NH, formalin (CH2O), oxalic acid (COOH) and copper sulfate pentahydrate.

Significant differences of the proposed method from the known.

The proposed method in contrast to the known allows to obtain (N,N'-tetramethylethylenediamine) copper sulfate pentahydrate (1) in one stage, without separation of the intermediate product (2) from the solvent using a rectification column at elevated temperature.

The method is illustrated by the following examples.

Example 1. In a glass (or metal) reactor, equipped with a mechanical stirrer, consistently load 2.05 mol 15% aqueous solution of dimethylamine, with stirring, 1.05 mol of formaldehyde, then slowly (not exceeding 20oC) 1 mol of 30% aqueous solution of oxalic acid and 1 mol CuSO45H2O, and stirred the reaction mass for 3 hours. Receive an aqueous solution of (N, N'-tetramethylethylenediamine) copper sulfate pentahydrate (1) with a yield of 99%. Exit (1) was determined after distillation of water at 40-42oC (100 Torr).

The spectral characteristics of the (N,N'-tetramethylethylenediamine) copper sulfate pentahydrate: IR spectrum (cm-1): 3540, 3320, 3230, 2930, 2860, 1680, 1660, 1440, 1380, 1110, 1020, 900, 860.

oC) and normal pressure.

A method of obtaining a (N, N'-tetramethylethylenediamine) copper sulfate pentahydrate General formula

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by reacting an aqueous solution of dimethylamine with formalin with the addition of an aqueous solution of oxalic acid and copper sulfate pentahydrate at a temperature of 21 - 22oC for 2 to 4 hours, wherein the molar ratio of the starting components is(2 - 2,1) : (1 - 1,1) : 1 : 1.

 

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