PL150335B1 - Method of obtaining aqueous solutions of n,n,n-trihydroxyethyl-n-stearylmethylenediamine hydrofluoride as well as of its mixture with oleilamine hydrofluoride - Google Patents

Description

PATENT DESCRIPTION

150 335

OFFICE

PATENT

RP

Additional patent to patent no-Pending: 87 10 16 / P. 280069 /

CVC priority

Int. Cl. ⁸ C07P215 / 18 A61K 7/18

Application announced: 88 07 07 Patent description published: ^{1990 10 31}

Creators of the invention: Marian Kajl, Wiesław Szelejewskl, Izabela Skrzypczak

Authorized by the patent: Institute of Pharmaceutical Industry,

Warsaw Poland/

METHOD OF PREPARING THE WATER SOLUTION OF THE HYDROGEN DIFLUORIDE MIXTURE

N, N, N * -TRIHYDROXYETHYL-N ^# -STEARYLTRIMETHYLENEDIAMINE WITH OLEILOAMINE FLUORIDE

The invention relates to a process for the preparation of an aqueous solution of a mixture of N, N, N'-trihydroxyethyl-N'-stearyltrimethylenediamine dihydrofluoride of formula 1 with oleylamine hydrofluoride of formula 2.

This solution is included in various cosmetic preparations, such as toothpastes, mouthwashes, etc., used prophylactically and therapeutically in tooth decay.

The method of preparing a compound of formula 1, known from German patent specification No. 1 198 493, consists in reacting an amine with a stoichiometric amount of hydrofluoric acid. The reaction was carried out as follows: approx. 20% water and 40% hydrofluoric acid were added to N, N, N * -trihydroxyethyl-N * -stearyltrimethylenediamine. The resulting pasty mass was homogenized by kneading and dried over water-extracting agents or in air. In contrast, the compound of formula 2 was obtained by treating a stoichiometric amount of 40% hydrofluoric acid on a methanolic oleylamine solution. Stripping the methanol gave a substance as a wax.

The compounds of formula (II) obtained in the known manner are in the form of a gel, a paste or a wax and are difficult to dissolve in water. The preparation of suitable solutions suitable for useable preparations encounters serious difficulties, especially since at certain concentrations these compounds have the ability to gel.

The method according to the invention produces an aqueous solution of a mixture of a compound of formula 1 with a compound of formula 2 by dosing the molten amine mixture heated to 60-65 ° C into an aqueous solution of hydrofluoric acid at a temperature of 5O -6O ° C and a concentration of not more than 3% at continuous intensive mixing.

150 335

The aqueous solutions obtained by the method according to the invention are convenient for use in the preparation of utility preparations, and are characterized by a high stability and can be stored.

The advantageous effect of the invention is to eliminate the need to use special equipment for mixing gelled bodies and organic solvents in the production process.

The following example illustrates the invention.

For example, To 2.63 kg of a 2.03% solution of hydrofluoric acid heated to 5O-6O ° C, a mixture of 0.562 kg of N, N, N * -trihydroxyethyl-N, heated to 60-65 ° C is gradually added with vigorous stirring. * -stearyltrimethylenediamine with 0.053 kg oleylamine. The resulting solution is cooled to room temperature. A 20% solution of a mixture of the compound of formula 1 and 2 is obtained.

Claims (1)

Patent claim A method of producing an aqueous solution of a mixture of N, N, N * -trihydroxyethyl-N * -stearyltrimethylenediamine dihydrofluoride with oleylamine hydrofluoride by reacting an appropriate amine with a stoichiometric amount of hydrofluoric acid, characterized in that the N, N mixture is melted and heated to 60-65 ° C The, N * -trihydroxyethyl-N'-stearyltrimethylenediamine with oleylamine is dosed into an aqueous solution of hydrofluoric acid at a temperature of 5O-6O ° C and a concentration not higher than 3%, with vigorous stirring, and the resulting solution is cooled to room temperature. ^H0 " ^C 2 ^H 4 \ HO-CgH / N ~ CH ₂ -CH ₂ -CH ₂ -N CgH ^ -OH / \ HF HF ^C 18 ^H 37 MODEL 1 PATTERN 2 Department of Publishing of the UP RP. Circulation 100 copies Price 1500 PLN