CS239115B1 - Method of 3-phenyl-1-propanol cleaning - Google Patents

Abstract

Amine impurities are subjected to the action of a solid acid adsorbent, preferably - alumina.

Description

The present invention relates to a process for purifying 3-phenyl-1-prepanel for perfumery purposes.

3-Phenyl-1-prepanol is an important synthetic fragrance. It is produced by the hydrogenation of cinnamylalkehel or cinnaaylaldehyde, which is only a minor step, by the hydrefermylation of styrene, which results in the formation of more or less precursors, or, to the greatest extent, the hydrogenation of 4-phenyl-1,3-diexane. 4-Phenyl-1,3-diexane is obtained in high yield by reaction from styrene and fermaldehyde, latices with acid catalysts, most often sulfuric acid. Work must be carried out with an excess of fermaldehyde, otherwise the yield of the low Pe reaction has to be neutralized and the excess formaldehyde, which would interfere with the distillation of 4-phenyl-1,3-diexane, must be destroyed. Most preferably, the reaction mixture is treated with ammonia feed to neutralize the sulfuric acid to form ammonium sulfate and react the fermaldehyde with ammonia to form urethra. These substances are then removed together with the scientific layer.

Such a treatment is sufficient to ensure that subsequent hydrogenation of 4-phenyl-1,3-diexane yields 3-phenyl-1-prepanel which, despite its rectification, has excellent analytical purity (99%). , has not been amine-containing substrates. Substances which also degrade the intrinsic properties of 3-phenyl-1-prepanel cannot even be removed by effective rectification.

This problem is reliably solved by a process for the purification of 3-phenyl-1-prepanel or 4-phenyl-1,3-diexane as an intermediate in the production of 3-phenyl-1-propanel according to the present invention, which is more particularly described above. The method according to claim 1, characterized in that the trace impurities of the amine nature will be treated with a solid acid adder and preferably with N-alumina. The most suitable arrangement is the reactor and the solid bed of the adserbent, which is sprinkled with kentamineven 4-phenyl-1,5-dioxane or 5-phenyl-1-prepanel, or it is gentle to survive even the powdered adserbent in a batch reactor β following separation.

The basic effect is to enhance the excellent inherent properties of 5-phenyl-1-prepanel.

The transition is evident from the following examples of a particular conversion.

Example 1

200 g of 5-phenyl-1-prepanel, a totally inefficient perfume site for a characteristic amine odor, was passed through the unactivated β-alunins. It was placed in a glass tube with a diameter of 20 mm, the height of the alignment was 200 mm, the grain was 0.2 mm, the amount of alumina was 50 g. The 5-phenyl-1-prepanel was collected at the outlet. to all requirements.

Example 2

It was peetupevan in the same manner as in Example 1 except that the purified raw material was 4-phenyl-1,5 * oxane. From this purified diexane, the product was prepared with excellent erganeleptic properties by means of hydrogenelysis.

Example 5

Purification of 5-phenyl-1-propanel resp. 4-phenyl-5-diexanu byle converted by mixing 5 g 2 ^{/ A 'AluI, II3} iy ¹⁰⁰ 8 organic substances.

After stirring for 2 hours, the catalyst was separated by filtration.

The effect of this cleaning method was the same as in Examples 1 and 2.

Claims (2)

Process for the purification of 3-phenyl-1-propanel or 4-phenyl-1,3-diexane as an intermediate in the preparation of 3-phenyl-1-propanel, characterized in that amine impurities are treated with a solid acidic adeorbent. , with benefit -aluainy. 2. A process according to claim 1, wherein the adsorption is carried out by mixing the solid adserbent with the contaminated organic matter in the liquid phase and separating it or by contacting the liquid and solid phase in a fixed bed reactor of the adserbent.