Researches on morphine. Pt. 1 / by S.B. Schryver and and Frederic H. Lees.

  • Schryver, S. B. (Samuel Barnett), 1869-1929.
Date:
[1900]
Catalogue details

Licence: In copyright

Credit: Researches on morphine. Pt. 1 / by S.B. Schryver and and Frederic H. Lees. Source: Wellcome Collection.

    10/20 (page 1031)
    a}f = - 4°26', 1=1 dcm., g — 1’65, [a]i>9°= - 268*6°. Examination of Mother Liquors from preparation of Chloromorphide, —After extracting the alkaline liquors with chloroform until nothing more went into solution, the aqueous residue always gave a fairly copious precipitate with Mayer’s reagent, and as the maximum yield of chloromorphide did not amount to more than 75 per cent, of the theoretical, a certain amount of another alkaloid must be present. The alkaline mother liquors were therefore carefully neutralised with dilute hydrochloric acid, and evaporated to a small bulk. On evapora¬ tion, the solution became acid, and more alkali was added from time to time to keep it perfectly neutral. The mixture was evaporated to dryness, and the residue extracted with absolute alcohol in a Soxhlet apparatus to separate the alkaloidal salt from the purely inorganic residue. After distilling off the alcohol, the residue was dissolved in water, the solution boiled with a little animal charcoal to decolorise it, made alkaline with sodium hydrogen carbonate, and extracted forty or fifty times with hot amyl alcohol. The base extracted in this way was removed from its amyl alcoholic solution by dilute hydrochloric acid, and the acid solution evaporated to a small bulk. When sufficiently concentrated, radiating clusters of long, silky needles commenced to separate out, in the form characteristic of morphine hydrochloride, and their identity with this salt was proved by a determination of the water of crystallisation. 0*9322 at 120° lost 0*1322 H20. H20=14*l. Cl7H1903N,HCl,3H20 requires H20 = 14*3 per cent. A bye-product therefore appears to be formed, which, on heating with water, is readily reconverted into morphine. This product has not yet been isolated. No trace of isomorphine could be detected. Acetylchloromorphide, Cll7H1702NCl,C0,CH3, can be prepared from chloromorphide by means of either acetic anhydride or acetyl chloride, the better result being obtained by the use of the latter. Chloro¬ morphide, mixed with about five times its weight of acetyl chloride, was heated for four or five hours on a water-bath in a reflux apparatus. The base nearly all dissolved. At the end of the reaction, the excess of acetyl chloride was distilled off, the residue dissolved in water, sodium carbonate added, and the base extracted with ether. On dis¬ tilling off the ether, the acetyl derivative remained behind, and was purified by recrystallising two or three times from absolute alcohol and finally from acetone. Acetylchloromorphide forms small, white, glistening plates, which soften at 173°, and melt at 174—178°, several recrystalhsations being required before a specimen can be obtained melting at the higher temperature.