DE431309C - Process for the continuous preparation of a mixture of camphene and isobornyl ester - Google Patents

Description

Process for the continuous preparation of a mixture of camphene and isobornyl ester. It is already a method of representing a mixture of camphene and isobornyl acetate from pinene chlorohydrate or containing pinene chlorohydrate Oil mixtures known (patent specification 2683o8).

The patent would have brought significant technical progress, if the dechlorine mixtures written in it after separation of the respective Terpene layer and the metal chloride concerned ride equal reaction force for further dechlorinations could have been used. The latter possibility is in the example 2 of the above patent, last paragraph, indicated.

It has been found, however, that the once used glacial acetic acid-zinc acetate mixture behaves differently than a freshly made one. The reaction lasts when you repeat Use of the dechlorine mixture longer, the yield of finished products is lower.

The cause of this phenomenon was found to be that the metal chlorides (with the exception of the zinc chloride which forms during the reaction), which in the first Use of fatty acid-fatty acid-zinc dishes to a certain extent remain dissolved in these, thereby delaying the course of the reaction and this too sometimes give a different direction. On the other hand, these reduce metal chlorides the condensing effect of the chlorine zinc formed in the reactions, so that the dechlorinations are carried out continuously with a small or even total no excess of fatty acid metal can begin.

The most varied attempts to continuously use the dechlorine mixtures according to patent 268308 while adhering to the time and yield specified in this patent did not lead to the goal.

Surprisingly, it has now been found that continuous work with one and the same dechlorination mixture while maintaining the high yields given in patent 2683o8 can be achieved in the same time if one uses such a lye regenerated in a known manner as the dechlorination liquor, which is already dechlorinating Has gone through temperatures above the boiling point of the fatty acids used, i.e. under pressure. Examples i. 172 parts of pinene chlorohydrate are mixed with 42o parts of a zinc acetate-glacial acetic acid solution that has already been used - consisting of 220 parts of glacial acetic acid, 125 parts of zinc acetate (anhydrous), 10 parts of \ atriutnacetat (anhydrous), about 50 parts of terpenes - in the autoclave. Heated to 10 to 1:25 'for hours, then 82 parts of anhydrous sodium acetate were added and the mixture was stirred for a further 1/2 hour at about 100 °. After several hours of marriage, the terpene layer separates out clearly. This is separated off, as is the precipitated sodium chloride, whereupon the zinc acetate-glacial acetic acid solution is ready for use again after it has been brought to the prescribed volume.

2. 72 parts of pinene chlorohydrate are mixed with 46o parts of a zinc acetate-glacial acetic acid solution that has already been used - consisting of 220 parts of glacial acetic acid, i25 parts of zinc acetate (anhydrous), one part of sodium acetate (anhydrous), about one part of sodium chloride and about 1 to 5 parts of terpenes. heated in the autoclave for 4 hours at 145 to r5o °. The further processing takes place as indicated under r.

Claims (1)

PATPNT-ANsPRUcii: Process for the continuous representation of a Mixture of camphene and isobornyl esters made from or containing pinene chlorohydrate Oil mixtures by heating with a fatty acid and fatty acid zinc, characterized in that that such a lye regenerated in a known manner is used as dechlorination liquor finds that already dechlorinations at temperatures above the boiling point of the applied Fatty acids lying down, i.e. under pressure.