SU3381A1 - Method for isolating codeine from opi - Google Patents

Description

P: Ri by: teaching morphine from opium by an alcohol-ammonia method, making it possible to isolate a high-grade technical base with a good yield, such a valuable alkaloid, like codeine, remains in the mother liquor, and its release is significant The technical difficulties that are caused by the presence of a large amount of basic and neutral resins accumulated in the mother liquor by extraction of opium and partly formed during the evaporation of the extract. But the ammonia ammonia method, which by its simplicity quickly gained a prominent place, was far from complete without isolating codeine.

The proposed method is to dispose of residues after separation of morphine according to the Patsukov method described in patent No. 127, with the least possible amount of solution for the crystallization of hydrochloric codeine, for which it is necessary to remove: 1) the resins are both neutral and basic; 2) associated alkaloids (papaverine, narcein and tebain) and 3) meconic acid.

To isolate the basic resins, the mother liquor, freed from alcohol, is diluted with water, and from the resins, it is decanted, and the alkaloids are extracted from it by adding amgiac to a distinctly odor. Together with alkaloids from A.miak, also resins that have not precipitated from the initial dilution with water fall out. After the separation of the alkaloids, the solution is heated for some time with lime to release the meconic acid, in the form of a calcium meconate, and after filtering, the meconatl is evaporated. One stripped off solution

acidified with hydrochloric acid and diluted with spirits. From the precipitated and precipitated resins, the alcohol solution is decanted, filtered, and the alcohol is distilled off. The residue after distillation of the alcohol is left for reinstallation.

Example. 100 kg of residues obtained after precipitation (10104) precipitates and freed from alcohol by distillation are diluted with an equal volume of water. A solution of ammonia and 25% of ammonia is added to a noticeable odor from the fallen out resin, and the solution is decanted into it, to free it from alkaloids and from non-diluted resins (until two operations can be combined): -And) the solution within 5 hours is processed with 5 kg of lime at 80 ° and good mixing. The precipitated calcium meconate is filtered off and the solution is evaporated with a volume of 20 liters. We will add that 2 kg of hydrochloric acid — beats — is added to the evaporated solution. at. 1.19 and 60 liters of 96 ° alcohol. The alcohol solution is drained from the precipitated and precipitated resins by decantation and alcohol.

as far as possible completely distilled. The residue for the separation of codeine hydrochloride is left to crystallize out, which lasts 2-4 days. The precipitated h.hydrohydrate is slightly diluted with alcohol. The output code is equal to 0.8% by weight of the extract; when the mothers stand for 3-5 days, more than 0.2% of codeine can be distinguished.

SUBJECT MATTER a.

The method of separating codeine from the op with preliminary treatment of the latter by the method described in patent 127, to isolate morphine, characterized in that the solution obtained from the extraction of morphine is removed by distillation of the alcohol by distillation with ammonia to remove tarry substances, and then processed with lime to remove meconic acid, the evaporated solution is evaporated to a small volume, diluted after acidification with strong alcohol to remove the residue of resinous substances, and finally, after removing the alcohol, salt is separated from the solution codeine by crystallization.