SU18746A1 - The method of obtaining eihinina - Google Patents

Description

otilugolnyy- ester quinine eyhinin is obtained usually action of ethyl chloroformate in rsnovakie in benzene solution (DRR №91370, Zimmer & C), for which purpose the first neobhodimd sulphate iln quinine hydrochloride translate the action of alkali in the base, or to suck on nuuche tsentrofuge , dried in a drying oven and for the final removal of the good in a vacuum dryer. These operations are associated with some loss of quinine, since quinine contains contaminants, the quinine base darkens somewhat during drying. Another method (DRP 118352, Zimmer & C) allows the use of dehydrated quinine salts, which is also associated with drying of hinium salts in a vacuum dryer. In the third method (DRP 123748, Zimmer & C °), conventional quinine salts, i.e., i.e., can be used. with crystallization water, but in this case pyridine must be added.

In the proposed method, the goal is to digest a benzene base solution

quinine, the salt of the latter is treated with an alkali solution in the presence of benzene. Thereafter, part of the benzene is distilled off from the solution along with the available water, and chlorofolic acid ethyl ester is added to the remaining solution and, at the end of the reaction, eiquinine is recovered in the usual way.

The method consists in the fact that the operation base for quinine is not separated separately, by independent operations in a dry, anhydrous state, but is obtained in a benzene solution immediately before the reaction of ethyl carbonate from quinine salt (sugate, hydrochloride) using treatment in the same benzene medium with aqueous alkali (ammonia, caustic soda, etc.), the subsequent separation of the aqueous layer from the benzene and the drying of the latter by distilling off a portion of the benzene.

The reaction is carried out as follows. The apparatus, which has a direct and reverse refrigerator, equipped with an outer jacket and a steam jacket, is loaded and loaded with quinine salt. Then when

During operation, the amount of alkali required for the transfer from the salt to the base is added and the mixture is heated under reflux to better dissolve the quinine base in benzene. The resulting ammonium sulfate or ammonium hydroxide (sodium) is converted into an aqueous solution, and the quinine base is benzene. The mixer is stopped, the liquids are separated and the aqueous solution of salt is drained through the lower valve. Since the benzene is wet, to remove water from the solution, some of the benzene is distilled off (switching the reflux cooler to direct). be muddy. The refrigerator is again switched back and the required amount of ethyl chloroforic acid is poured into the benzene solution of the quinine base. On the following day, eichinine hydrochloride is sucked off, washed with benzene Kusushat, and the base is subsequently transferred to eikhinin, usually by, i.e. precipitation with alkali. /

/

The subject of the patent.

The method of obtaining eichinine, characterized in that the quinine salt is treated with an alkali solution in the presence of benzene, in order to obtain a benzene solution of the quinine base, then part of the benzene is distilled off from the benzene solution together with the water contained in the solution, after which ethyl chloroforic acid ester is added to the solution at the end of the reaction, eichinin is recovered from the product obtained in the usual way.