The method of producing complex magnesium bonds

 

(57) Abstract:

The invention relates to the field of organic chemistry, specifically to an improved method of obtaining Mdtp. MTAP can be used as intermediate for the preparation of catalysts of oxidation-reduction reactions and polymerization reactions in the manufacture of dyes and semiconductors. The objective of the invention was to develop a method of obtaining MTAP, allowing to increase output, reduce the overall time of the process, to eliminate the preliminary drying of the solvent. The problem is solved by a method of obtaining Mdtp by the interaction of dinitrile maleic acid with magnesium alcoholate in an environment of an organic solvent, in which as magnesium alcoholate using 1-butyl magnesium, and as an organic solvent using 1-butanol and the process is carried out at a slow heating of the reaction mixture from 25 to 90oFrom within 50-70 minutes 1 Il., table 2.

The technical field.

The invention relates to the field of organic chemistry, specifically to an improved method of obtaining Mdtp. MTAP can be used as intermediate for the preparation of catalysts of oxidation-vosstanovitelya.

A method of obtaining MDAP interaction succinimides and formate in organic solvents boiling [Elvidge, G. A., R. P. Linstead// J. Chem. soc. , 1953, p. 3536-3544]. The maximum yield of 3%. The disadvantages of this method are the low yield of the final product and high consumption of the starting materials.

The closest technical solution is a method for MTAP interaction dinitrile maleic acid with 1-propietor magnesium [Linstead, R. P. , Whalley M.// J. Chem.Soc., 1952, p. 4839-4846]. The process is carried out at boiling (temperature 98oC) in 1-propanol for 17 minutes. Output MDAP ranges from 2 to 15% (average 8%). Source 1-propilot magnesium is produced by boiling magnesium in 1-propanol for 6-7 hours. The reaction is initiated with a small amount of iodine. 1-propanol is pre-dried by distillation over metallic sodium. The disadvantage of this method is the low yield, the long duration of the stage 1-propylate magnesium, additional phase dehydration of 1-propanol.

The essence of the invention.

The objective of the invention was to develop a method of obtaining MTAP, allowing to increase output, reduce the overall time of the process (including the stage of dehydration of 1-propanol and prigotovlen to provide a method of obtaining MDAP interaction dinitrile maleic acid with a suspension of 1-butyl magnesium in the environment of 1-butyl alcohol at slow heating of the reaction mixture from 25 to 90oC for 50-70 minutes.

The process is carried out as follows. Source 1-butyl magnesium is produced by boiling magnesium in 1-butanol for 1-3 hours, and to activate the reaction of formation of 1-butyl magnesium add separate portions of a saturated solution of iodine in 1-butanol, pre-heated to the boil. The resulting suspension of 1-butyl magnesium in 1-butanol is cooled to 25oC, add dinitrile maleic acid and slowly heated the reaction mixture is from 25 to 90oC for 50-70 minutes. Output MDAP 25-30%.

Information confirming the possibility of carrying out the invention.

Example 1.

To 1 g of magnesium was added 10 ml of 1-butanol, heated to boiling and 20 ml was added within 15 min, a saturated solution of iodine in 1-butanol. The mixture is boiled under stirring for 2 h the resulting suspension of 1-butyl magnesium in 1-butyl alcohol is cooled to 25oC and add 4 g of dinitrile maleic acid. Thus there is a faint yellow-brown colour. The reaction mixture is heated for 30 min from 25 to 75oC, with its color gradually changes and becomes intensely green. Heating continued for another 40 minutes, increasing temperature is a purple tinge. After that the reaction mixture is cooled, the solvent is removed by distillation in vacuo, the residue is extracted in to conventional Soxhlet extractions at first with benzene to remove impurities, then with methanol. The solvent is removed, to obtain 1.2 g MDAP (30%).

The data of elemental analysis of the obtained product:

Found, %: 57,42 C; 33,10 N; 2,20 H.

CHNMg

Calculated, %: 57,14 C; 33,30 N; 2,38 H.

Absorption spectra of the obtained product:

in methyl alcoholmax(): 332 (4,70), 584 (5,03);

in pyridinemax(): 332 (4,60), 540 (4,14), 587 (5,07).

The clean lines of the infrared spectrum of the obtained product are shown in table. 1.

Examples 2, 3, 4, 5, different from example 1 temperature and duration of the process, are given in table. 2.

Thus, the proposed method for MTAP allows to solve the problem of the invention, i.e. to increase the yield of 25-30% compared with 2-15% in the prototype), to reduce the total, including the stage of preparation of the magnesium alcoholate, the process (2 to 4 hours compared to 6 to 7 hours in the prototype), to eliminate the preliminary drying of the solvent.

The method of producing complex magnesium bonds by the interaction of dinitrile maleic acid with alcoh the comfort of 1-butyl magnesium, and as an organic solvent using 1-butanol and the process is carried out at a slow heating of the reaction mixture from 25 to 90oWith over 50 - 70 minutes

 

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