Researches on morphine. Pt. 2 / by S.B. Schryver and Frederic H. Lees.

  • Samuel Barnett Schryver
Date:
[1901]
Catalogue details

Licence: In copyright

Credit: Researches on morphine. Pt. 2 / by S.B. Schryver and Frederic H. Lees. Source: Wellcome Collection.

    15/22 (page 575)
    This substance was extremely soluble in water, giving a strongly alkaline solution, which proved to be free from silver, iodine, sulphuric acid, and barium. The powdered substance was dissolved in hot methyl alcohol, excess of methyl iodide added, the solution boiled for half an hour on the water-bath, and then concentrated, when a beautifully crystalline methiodide separated. This was collected and dissolved in hot methyl alcohol, in which it was easily soluble, but separated readily on cooling in the form of glistening leaflets melting at 262° with de¬ composition. On analysis, the following results were obtained : 0-1614 gave 0-3042 C02 and 0*0826 H20. C = 51*4; H = 57. 0-4529 required 10-4 c.c Nj 10 AgN03 solution. 1 = 29-1 Ci9H2403NI requires C = 51*7 ; H = 5-5; I = 28-8 per cent. A determination of the specific rotation in aqueous solution gave the following result: aD= — 2°30'; 1=1 dcm. ; c = 2-504; [a]JT= -99*8°. woCodeine methiodide is nearly insoluble in hot ethyl alcohol, but readily soluble in hot water, and on concentrating the solutiou, separates in a beautifully crystalline form. When its solution in dilute sodium hydroxide is boiled for two minutes, the clear liquid quickly becomes clouded with oily drops, soon solidifying to a crystal¬ line mass, which, after recrystallisation from alcohol, melts at 167°. The preparation of this base from fsocodeine methiodide is described in detail on p. 577. (b) By the action of Sodium Ethoxide and Methyl Iodide on isoMor¬ phine.— fsoMorphine (5*25 grams) was suspended in ethyl alcohol, and a solution of sodium (0-42 gram = 1 atomic proportion) in alcohol slowly added, with shaking. The fsomorphine went into solution, forming a sodium derivative. Methyl iodide (10 grams) was then added, and the solution boiled for 20 minutes, when suddenly a crystalline methiodide separated in quantity. This was collected and found to melt at 265°, with decomposition. A determination of the specific rotation in aqueous solution gave the following result: aD= -2027'; 7=1 dcm.; c = 2-40; [a]iT= -102*1°. This methiodide was in all respects identical with the one prepared by method (a), yielding, on boiling its aqueous solution with sodium hydroxide, the base melting at 167°. (c) From Codeine. Bromocodeide, C18H20O2NBr.—Codeine dried at 100° (24 grams) was dissolved in chloroform (60 grams) contained in a reflux apparatus, and phosphorus tribromide (24 grams), dissolved in about an equal weight of chloroform, was added. Immediate inter¬ action took place with development of heat and evolution of some