CS215216B1 - Method of making the thebain - Google Patents

Description

The present invention relates to a further development of the invention according to the Czechoslovak author's certificate No. 214902, the object of which is a method for producing thebaine from Papaver bracteatum Lindl, in particular roots and / or de-capped capsules. The principle of this process is that the starting crumbled dry drug is extracted, preferably by percolation, at 15 to 40 ° C, with an aromatic hydrocarbon, after alkalization with an aqueous solution of ammonia, an alkali metal hydroxide or carbonate or an aqueous suspension of an oxide or an alkaline earth metal hydroxide. C 6 -C 8, preferably toluene, in a weight ratio of 6: 1 to 12: 1, based on the weight of the starting drug, whereupon the extract is evaporated, and the thebaine is isolated from the residue as the hydrogen tartrate.

A further improvement of the cited author certificate is the process for producing thebaine according to the invention, characterized in that the starting drug is extracted with an aromatic hydrocarbon having 6 to 8 carbon atoms, preferably toluene, in a weight ratio of 4: 1 to 12: 1, preferably 5: 1 to 7: 1, based on the weight of the starting drug, after which the extract obtained is evaporated at a pressure of 1300 to 14000 Pa to 1/25 to 1/100 of the original volume and the thebaine crystalline base is isolated from the residue.

Further experiments have shown that, especially on a larger scale, thebaine in crystalline form as a base can be easily isolated directly from the concentrated extract, i.e. without the need for evaporation to dryness and without isolation of thebaine contained in the hydrogen tartrate evaporator. By cooling the residue, representing about 1/25 to 1/100 of the original extract 'j166, the very pure thebaine base crystallizes readily, uniformly chromatographically in good yield. Even the second product, obtained from the concentrated mother liquor after isolation of the first product, is very pure and usable together with the first product for further processing, i.e., to be converted into any desired salt or to the desired chemical transformation.

The mother liquors after repeated concentration and suction of the second crop can be isolated by residual thebaine by conversion into mineral or organic acid solutions, alkalization and extraction of the alkaline solution with toluene to give thebaine from the extract of this extract, which is purified preferably in the form of hydrogen tartrate.

The process according to the invention is more economical than the process according to the basic author's certificate No. 214902, because it is possible to work with smaller volumes of toluene, the extract does not need to evaporate to dryness and in case of further processing it is not necessary to release and isolate the base by decomposition of hydrogen tartrate. This will save the excipients, the solvent, the "device, and the

Further details of the method according to the invention can be seen from the examples.

EXAMPLES Example 1

Mix 10 kg of dry ground roots of petiolus bncteatum Lindl well in a large container. (0.79 x tru.ot, thebaine in sudine, loss on drying 6.6 liters by weight) $ e 60Cg chamber lime hydrate (69.4 liters by weight of calcium hydroxide) (and the mixture is then moistened by successive mixing by adding 2 / CO ml of water (25 < -1 > by weight of drug). The mixture is left in the culture over o.oc and then percolated with toluene at a rate of 10 liters / hour. The weight ratio of drug-solvent is about 1: 4 to about 1: 7. The combined toluene extracts are thickened at a pressure of about 10 660 la no 1/70 to 1/100 of the original volume. The crystalline base of thebaine, which is washed 3 times with suction, washed with a small amount of toluene and dried at room temperature, is cooled down to 50 DEG C. The residue is slightly beige in color, is practically uniform by chromatography and lays at. 2.6 DEG C. by purification of the mother liquor The second portion was washed with toluene, and was of two qualities to be deposited from the main portion, mp, 1 °, 5 ° to 17 °, 5 ° C. The newt yields 7d, 1 g of thaboin base. Example 2

In a large scale, wells of dry ground poppy seed mixed with fapaver bracteatum linul (1.074 wt.% Of thebain in dry matter, loss; drying 9.7 wt.%) Mixed with 2 The lime hydrate (containing 69.4% by weight of calcium hydroxide) was added to the mixture, and the mixture was then moistened with the gradual addition of 7.5 liters of water while stirring. The swollen and homogeneous olcan-encapsulated drug is left overnight and then poured into a percolator into which 80 to U'5 liters of toluene are introduced and the percolstor is supplemented with toluene so that all the drug is immersed. After standing overnight, the drug was percolated with toluene at a rate of 10 liters of extract per 30 min. The weight ratio of dcoga-solubility is between 1: 5 and 1: 7. The intoxicated toluene extracts are concentrated from a Llux of 13p3 to 10660 Pa to 1/25 to 1/50 'of the original volume «from the concentrated extract to be cooled», the first part of the crystalline base of thebaine being precipitated. The product is filtered off with suction and freed from chlorophyll several times by trituration. By concentrating the toluene mother liquors, a second portion of thsbain base is obtained, which is also refined by stirring several times with petroleum ether. A total of 316.1 g of thebaine is obtained in both proportions, which is only slightly beige in color and is uniform in chromatography. Mp.1-196-197 ° C. The second fraction is 191-194 ° C.

Claims (1)

Method of production of thebaine according to CS. No. 214902, characterized in that the starting drug is extracted with an aromatic hydrocarbon having 6 to 8 carbon atoms, preferably toluene, in a weight ratio of 4: 1 to 12: 1, preferably 5: 1 to 7: 1, based on weight of the starting drug, then the extract obtained is evaporated at a pressure of 1300 to 14000 Pa to 1/25 to 1/100 of the original volume and the crystalline base of thebaine is isolated from the residue.