The method of obtaining sodium or potassium salts of acids orthocarbonate

 

(57) Abstract:

Usage: as intermediates in organic synthesis and in the printing industry. Entity: an improved method of obtaining sodium or potassium salts of orthocarbonic acids of the formula R-C(OMe)2(OH), where Me is Na, K; R is phenyl, furyl, R1-CH=CH - - CH3(CH=CH)2- -, , R1- phenyl, furyl. Reagent 1: potassium salt of the carboxylic acid of the formula R - (OMe)C = O, where R and Me have the specified values. Reagent 2: an aqueous solution of sodium hydroxide or potassium hydroxide with a concentration of 6 to 8 mol/l reaction Conditions: reagent 1 is treated with reagent 2 adding an organic solvent is diethyl ether in a volume ratio diethyl ether: reaction mass is equal to (1,95 - 2,05) : 1, and the process is conducted at room temperature, remove excess alkali, at a molar ratio of the alkali salt of carboxylic acid (4 - 0,5) : 1 and the alkali concentration not lower than 5 N. in the reaction solution.

The invention relates to new methods of obtaining salt orthocarbonate acids or alcoholate hem-triolo having the structural formula R-Me where R is phenyl, furyl, R1-CH= CH-, CH3-(CH= CH)2- CH= C-CH3; Me - Na, K; Rlis phenyl, furyl, used as Premiata is a method of obtaining salts orthocarbonate acids by the interaction of organic acids with the alkali in the two-phase system dioxane - concentrated alkali, designed primarily to obtain potassium ortofrutticoli acids. Closest to the claimed is a method consisting in mixing a concentrated aqueous alkali with a heterogeneous mixture of organic carboxylic acid - water (Shapiro Y. M . Journal of General chemistry, 1988, I. 58, No. 4, S. 987). In both cases, the product is formed by the following reaction: R-O R - R-Me

The disadvantage of this analog is used as the initial reactant carboxylic acid in a heterogeneous conditions can lead to the formation of a product containing as impurities of unreacted alkali and salt of carboxylic acid formed as an intermediate reagent.

The aim of the invention is the provision of a more pure product by adnotatione education orthocarbonate acids, as well as the availability orthocarbonate salts through the use of industrially produced chemicals, and the use of more efficient way to extract the product from the reaction mixture.

This goal is achieved by the fact that as one of the initial reagents are taking sodium or potassium salt of carboxylic acid is H with a concentration of 6-8 N. so that the total mass of the mixture created the lye concentration not lower than 5 N. , and after the formation of a copious precipitate orthocarbonate salt in the reaction mixture at room temperature, add diethyl ether at 2 0,5 exceeds the volume of the reaction mixture. The total concentration of alkali for a complete product education should exceed the amount of salt carboxylic acid 4 0.5 times. As a result of these operations orthocarbonate salt is transferred from the aqueous-alkaline phase in the phase diethyl ether, forming a heterogeneous suspension, which is shared by known methods. For example, crystals of Articoli can be separated by centrifugation or by filtration on a glass filter under vacuum water pump. Then the white crystalline product is dried in a thermostat at 40-50aboutC for 2 h and examined for purity.

The quality of the product and its identification are flame photometric determination of the percentage content of sodium or potassium, elemental analysis, IR-spectroscopy in the presence of a bandhe3800 cm-1, potentiometric titration of a sample of salt dissolved in water.

P R I m e R 1. Dinitrourea terasawa 24 g (0.6 M) of NaOH. The resulting viscous mass is then cooled to 15-20aboutWith and poured 200 ml of diethyl ether. After 1 h the mixture splits into the bottom layer, containing an aqueous solution of excess alkali, and the top representing heterogeneous mixture orthocarbonate salt in the air. Lower alkaline layer is removed using a separating funnel or a suction pipette, and the upper transferred to a glass filter and under the action of the water jet pump broadcast press, and the product after repeated washing with ether, dried in a thermostat at 40-50aboutC. the Obtained white crystalline product (27 g or 98% ). Potentiometric titration of an aqueous solution of Nevsky product installed purity of 98% . Flame photometric method set the sodium content of 24.6% (Calculated - 25% ). Here is the chemical equation for the formation of this product + NaOH __ Na

P R I m m e R 2. Denationalised. In 50 ml of water is dissolved to 14.4 g sodium benzoate (0.1 M) and poured 50 ml of an aqueous solution containing 20 g (0.5 M NaOH. Then proceed as described in example 1. Ether is added in the amount of 220 ml Yield 98% (18.0 g).

Similarly, with the release of 96-99% receive orthocarbonate salt on the basis of NaOH and KOH for the rest orthocarbonate acids, of these structures.

Journal of General chemistry 58 No. 45, 1988, S. 987.

The METHOD of OBTAINING SODIUM OR POTASSIUM SALTS of ORTHOCARBONIC ACIDS of General formula

R-Me

where Me is Na, K;

R is phenyl, furyl; R1-CH= CH-, CH3(CH= CH)2-, CH2= C-CH3where R1is phenyl, furyl,

processing oxygen-containing compounds with an aqueous solution of sodium hydroxide or potassium hydroxide with a concentration of 6-8 mol/l at room temperature with the addition of an organic solvent and removing excess alkali, characterized in that as the oxygen-containing compounds using sodium or potassium salt of the carboxylic acid of General formula

R-/

where R and Me have the specified values,

as the solvent used diethyl ether in a volume ratio diethyl ether: reaction mass of 1.95-2.05 is: 1 and the process is conducted at a molar ratio of the alkali salt of carboxylic acid is 4 to 0.5 : 1 and the alkali concentration not lower than 5 N. in the reaction solution.

 

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