The method of obtaining pinacoline

 

(57) Abstract:

Use to get pinacoline. The inventive method of producing pinacoline includes processing 2,3-dimethylbutadiene-1,3 3 - 35% solution of sulfuric acid or 10 - 40% solution of methylphosphonic or 30 - 60% solution diphosphonic acid, or 5 - 30% acid salts of alkaline metal of this acid or mixtures of these acids and their salts at a temperature of 70 - 170oC, followed by separation of the medicinal product. table 2.

The invention relates to the chemistry of ketones, and in particular to methods of obtaining pinacoline.

In industry pinacolin used as a solvent for paints, inks, is an intermediate in the synthesis of medicinal and aromatic substances, pesticides group triazines and others.

The literature describes a number of methods of getting pinacoline. For example, pinacolin you can get pinacoline and similar rearrangements of enconcert with the release of 80-90 %, the interaction of the acid chloride trimethylhexanoic acid with organic (zinc, tin) compounds with yields up to 80 %, by the interaction of esters with magnetogenesis compounds in the presence of a complex catalyst, vidiocon solvents, output 32-58 %, the recovery of oxide mesityl zinc in a solution of sodium hydroxide or potassium in the presence of copper salts as catalyst, the yield of about 58 %. Pinacolin can also be obtained by methods based on the reaction of the Prince, namely, the interaction of isoamylenes or derivatives thereof with formaldehyde or its derivatives in the presence of catalysts. Most of these methods, due to low availability and high cost of reagents, the complexity of processes and other reasons, are only of theoretical interest.

Closest to the invention is a method for pinacoline interaction of 2,3-dimethylbutene-2 with formic acid and hydrogen peroxide in the medium of sulfuric acid and in the presence of nitrogen-containing catalyst.

However, this method is characterized by low (60%) yield of the target product and a large amount of wastewater, which are formed during the neutralization of spent catalyst.

The aim of the invention is to increase the yield of the target product and the elimination of sewage.

The objective is achieved by the fact that as a source of unsaturated hydrocarbons using 2,3-dimethylbutadiene-1,3, t in the environment in the recycling 5-60 % aqueous solutions of sulfuric, phosphoric, phosphonic or diphosphonates acids or 5-30 % aqueous acidic alkali metal salts of these acids or mixtures of these acids and their salts. The initial concentration of aqueous solutions of catalysts support the addition of water. Aqueous solutions of acids, salts and mixtures thereof are used in the process for a long time.

The proposed method allows to obtain the target product with the release of 93-98 %, excluding wastewater generation. The process is simple in hardware design and can be carried out in a continuous execution.

Example: In a vial with a capacity of 15 ml load 6 ml of an aqueous solution of catalyst and 4 ml of 2,3-dimethylbutadiene-1,3. The ampoule is sealed, immersed in a thermostat at a temperature of 70-170oC, then after 5 min include a vibrator. Every 5 min shaking the ampoule disconnect from the vibrator, cool and analyze the organic layer. The analysis is performed on the chromatograph Color with a flame ionization detector. Sorbent 10 % polyethylene glycol PEG-6000 on chromaton N - AW (0,25-0,315).

Column length of 2 m, diameter 4 mm

The volume of the sample 1 μl.

Upon reaching the maximum degree of conversion of 2,3-dimethylbutadiene-1,3 organic layer is shipped with the results summarized in table.1.

Examples of the durability of the catalyst are given in table.2.

Thus, the proposed method has significant advantages in comparison with prototype:

allows to obtain a product with high (93-98 %) output and virtually eliminate wastewater generated.

As a base case adopted a method of producing pinacoline electrochemical dimerization of acetone with subsequent rearrangement (19,5). The output pinacoline on the acetone is 48 %. On 1 t of the target product when the play method is formed of 16 m3wastewater and 1.4 m3organic waste.

The method of obtaining pinacoline, including the processing of unsaturated compounds in the presence of an acid, characterized in that, to increase the yield of the target product, 2,3-dimethylbutadiene-1,3 treated with 3 - 35% solution of sulfuric acid or 10 - 40% solution of phosphoric acid, or 20 to 50% solution of methylphosphonic or 30 - 60% solution diphosphonic acid, or 5 to 30 wt.% acidic alkali metal salt of this acid or mixtures of these acids and their salts at 70 - 170oWith subsequent isolation of the target product.

 

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